Reaction kettle for reaction preparation of diethyl acetamidomalonate

Abstract

The reaction kettle for the reaction preparation of the diethyl acetamidomalonate comprises a kettle body, a raw material dropwise adding assembly, a linkage structure, a stirring structure and an auxiliary cooling assembly. In order to solve the problems that when an ordinary reaction kettle is used for oximation reaction in diethyl acetamidomalonate reaction preparation, the reaction is violent and the reaction is not uniform and insufficient due to the fact that raw materials are mixed at a time, a raw material dropwise adding assembly is designed, the raw materials can be conveniently and gradually dropwise added into a kettle body through the raw material dropwise adding assembly, and the reaction efficiency is greatly improved. The reaction can be carried out step by step, the problem that the reaction is too intense is avoided, further, a stirring structure is designed, and automatic stirring and mixing can be carried out through the stirring structure during the reaction, so that the reaction is sufficient.

Description

Technical Field

[0001] The present application relates to the technical field of chemical reactors, in particular to a reactor used for the reaction preparation of diethyl acetamidomalonate. Background Art

[0002] Diethyl acetamidomalonate is also known as α-acetamidomalonate, with a molecular formula of C9H15NO5. In the preparation of diethyl acetamidomalonate, diethyl malonate is obtained by nitration, reduction and acetylation of diethyl malonate. In the process, the oximation reaction to convert diethyl malonate into diethyl nitrosomalonate is a key step. This conversion is a prerequisite for the subsequent reductive acylation reaction and is crucial to the formation of the final product. When performing the oximation reaction, the corresponding reactor is required.

[0003] There are various reactors in the prior art, such as horizontal kneading reactors, which have large reaction volumes, excellent mixing performance, surface renewal performance, heat transfer performance and self-cleaning performance, and thus have broad application prospects in the fields of bulk polymerization, condensation polymerization and polymer devolatilization. However, the kneading reactor has a very complex geometric structure, and the experimental measurement technology has great limitations. The reactor for oximation reaction in the prior art usually includes a reactor, a rotating shaft and a sealing device for the reactor. This reactor involves a spiral seal, a sealing ring and a sealing shell, so it is usually used to form a space suitable for accommodating the spiral seal and the sealing ring. There is also a horizontal alkylation reactor in the prior art, which has been treated with anti-corrosion and has thickened tube walls, which can effectively alleviate the corrosion of sulfuric acid to the heat exchange tubes and extend the service life of the tube bundle. The reactor is usually composed of a shell, an inner tube, a tube bundle and a tube box, and at least one anti-corrosion layer is provided on the inner wall and the outer wall of the tube bundle.

[0004] Existing Chinese patent document CN221674272U discloses a reactor for oximation reaction, which can perform nitration reaction for the preparation of diethyl acetamidomalonate. However, during the reaction, since the nitration reaction releases a large amount of heat, adding the raw material solution at one time is likely to produce a violent reaction, resulting in rapid temperature rise and causing dangerous problems. At the same time, the stirring structure of the reactor is usually fixed-rate stirring. During the raw material addition process, it is easy to stir relatively quickly to generate a large amount of foam or stir relatively slowly to cause insufficient reaction.

[0005] That is, the reactors for nitration reaction in the prior art generally have the problem of rapid internal temperature rise during the nitration reaction, which may cause danger.

[0006] For example, Chinese patent document CN219291429U discloses a reactor, which includes a main body structure, a diversion structure including a diversion hood, etc. The reactor can effectively enhance the reaction between various raw materials in the preparation process. However, the reactor cannot effectively prevent dangerous problems caused by excessively rapid temperature rise inside the reactor.

[0007] There is an urgent need in the prior art for a reactor for preparing diethyl acetamidomalonate that can safely perform a nitration reaction. Summary of the invention

[0008] In view of the technical problems existing in the prior art, the present invention aims to provide a reactor for the preparation of diethyl acetamidomalonate, which can prevent the rapid internal temperature rise of the reactor during the nitration reaction and cause danger.

[0009] According to one aspect of the present invention, a reactor for preparing diethyl acetamidomalonate is provided, comprising: A kettle body, wherein the kettle body is fixedly arranged on the upper surface of the fixed base, a kettle cover is fixedly connected to the upper end of the kettle body, and the kettle body is used for oximation reaction; A raw material dropping component, the raw material dropping component is fixed to the side wall of the fixed plate frame, the fixed plate frame is fixedly arranged on the upper surface of the fixed base, and the raw material dropping component is used to gradually drop the raw material solution; A linkage structure, wherein the linkage structure is fixedly arranged on the top of the fixed plate frame, and the bottom end of the linkage structure is connected to the raw material dripping assembly; A stirring structure, wherein the stirring structure is arranged on the kettle cover and is used for automatically rotating and stirring during the oximation reaction; The auxiliary cooling component is fixedly arranged at the bottom end of the stirring structure, and is used for automatically cooling during the oximation reaction.

[0010] Furthermore, the raw material dripping assembly includes a movable slider, a rotating disk, a rocker, a servo motor, a fixed tripod, a fixed cylinder, a movable piston, a movable guide rod, an output hose and an input pipe. A guide groove is provided at the fixed plate frame, and a movable slider is slidably connected to the guide groove. A rotating disk is rotatably connected to a side wall of one side of the fixed plate frame, one end of a rocker is rotatably connected to the side wall of the rotating disk, and the other end of the rocker is rotatably connected to the side wall of the movable slider. A servo motor is fixedly connected to the other side of the fixed plate frame, and the end of the output shaft of the servo motor is fixedly connected to the rotating disk.

[0011] Furthermore, the fixed tripod is fixedly arranged on the side wall of the fixed plate frame, and a fixed cylinder is fixedly connected to the upper surface of the fixed tripod, and a movable piston is slidably connected in the inner cavity of the fixed cylinder, and one end of a movable guide rod is fixedly connected to the upper surface of the movable piston, and the other end of the movable guide rod penetrates the upper wall of the inner cavity of the fixed cylinder and extends outside the wall, and the top of the movable guide rod is fixedly connected to the movable sliding block, and one end of an output hose is fixedly connected to the bottom side of the inner cavity of the fixed cylinder, and the other end of the output hose extends to one end of the feed pipe and is fixedly connected to the feed pipe, and an output check valve is installed on the output hose, and an input pipe is fixedly connected to the bottom side of the inner cavity of the fixed cylinder, and an input check valve is installed on the input pipe.

[0012] Furthermore, the linkage structure includes a fixed cross plate, a guide rod, a connecting plate, a rack, a connecting rod, a fixed seat, a rotating rod, gear A, a bevel gear A, a rotating rod, gear B and a bevel gear B. The fixed cross plate is fixedly arranged on the side wall of the fixed plate frame, and the fixed cross plate is slidably connected with the guide rod. The upper and lower ends of the guide rod are fixedly connected with connecting plates, and one end of the connecting rod is fixedly connected to the connecting plate on the bottom side, and the other end of the connecting rod is fixedly connected to the movable slider. A rack is fixedly connected between the two connecting plates, and the rack passes through the fixed cross plate.

[0013] Furthermore, a fixed seat is fixedly connected to the upper surface of the fixed horizontal plate, a rotating rod is rotatably connected to the fixed seat, a gear A is fixedly connected to one end of the rotating rod, the gear A and the rack are meshed with each other, a bevel gear A is fixedly connected to the other end of the rotating rod, a rotating rod is rotatably connected to the fixed horizontal plate, a bevel gear B is fixedly connected to the upper end of the rotating rod, the bevel gear B and the bevel gear A are meshed with each other, and a gear B is fixedly connected to the bottom end of the rotating rod.

[0014] Furthermore, the stirring structure includes a stirring shaft, a stirring blade, a gear C and a rotating joint. The stirring shaft is arranged at the kettle cover and is rotatably connected to the kettle cover. The bottom end of the stirring shaft is fixedly connected to the stirring blade, and the upper end arc wall of the stirring shaft is fixedly connected to the gear C. The gear C and gear B are meshed with each other.

[0015] Furthermore, an inner cavity is provided inside the stirring shaft, and a rotating joint is fixedly connected to the upper end of the stirring shaft.

[0016] Furthermore, the auxiliary cooling component includes a fixed shell, a heat-conducting roller, a connecting pipe A, a connecting pipe B, a rotating shaft, a baffle, a circular fixed shell, a clockwork spring, an ice water bin and a pump. The fixed shell is fixedly arranged on the arc wall of the stirring shaft, and a plurality of heat-conducting rollers are fixedly arranged in the inner cavity of the fixed shell. A connecting pipe A is fixedly connected between the plurality of heat-conducting rollers, one end of a connecting pipe B is fixedly connected in the inner cavity of the stirring shaft, and the other end of the connecting pipe B is fixedly connected to the heat-conducting roller.

[0017] Furthermore, ice water is arranged in the inner cavity of the ice water bin, a pump is fixedly connected to the upper surface of the ice water bin, the input end of the pump is fixedly connected to one end of an input pipe, the other end of the input pipe extends into the ice water, the output end of the pump is fixedly connected to one end of an output pipe, and the other end of the output pipe is connected to a rotary joint.

[0018] Furthermore, a rotating shaft is rotatably connected to the openings on both sides of the fixed shell, a baffle is fixedly connected to the arc-shaped wall of the rotating shaft, a circular fixed shell is fixedly connected to the upper surface of the fixed shell, one end of the rotating shaft extends into the inner cavity of the circular fixed shell, one end of a clockwork spring is fixedly connected to the inner cavity of the circular fixed shell, and the other end of the clockwork spring is fixedly connected to the rotating shaft.

[0019] It should be noted that in actual preparation, four reactors of the present invention are usually used side by side for oximation reaction. And as a feeding method, it is preferred to design a sodium nitrite dissolving kettle separately to dissolve sodium nitrite, design a barrel structure separately to contain diethyl malonate and process water, and use a diaphragm pump to pump diethyl malonate into the dissolving kettle. Since it does not belong to the gist of the present invention, it is not described in detail.

[0020] The auxiliary oximation synthesis feeding method of the present invention may include the following steps: 1. Use a diaphragm pump to input 800kg barrels of process water into the sodium nitrite dissolving kettle; 2. Open the dissolving kettle cover and put 200kg sodium nitrite into the kettle; 3. Use a diaphragm pump to input 400 kg of diethyl malonate into the dissolving kettle; 4. Start stirring the dissolving kettle, stir for 30 minutes, then open the bottom valve of the dissolving kettle and put the materials in the dissolving kettle into the designated oximation reactor; 5. Pump 184 kg of glacial acetic acid into the high-level tank and add it dropwise.

[0021] According to the present invention, since the raw material dropping component can conveniently drop the raw materials into the kettle body step by step, so that the reaction can be carried out step by step, the problem of overly intense reaction can be effectively avoided. Furthermore, the present application has designed a special stirring structure, through which the stirring structure can automatically stir and mix during the reaction, so that the reaction is sufficient. At the same time, in conjunction with the setting of the linkage structure, the stirring rate can be automatically adjusted according to the rate of dropping the raw materials, without the need for an additional power source, which solves the problem that the stirring structure of the ordinary reactor in the prior art has a constant speed, and the reactants are slowly added, which is prone to stirring relatively quickly to produce a large amount of foam or stirring relatively slowly to cause insufficient reaction. At the same time, the present application has set up an auxiliary cooling component, through which the temperature in the oximation reaction process can be cooled and controlled, avoiding dangerous situations caused by excessively high temperatures during the reaction process. At the same time, the cooling rate can be automatically controlled in conjunction with the stirring speed, and the phenomenon of too low temperature of the reactants due to excessive cooling is avoided, achieving a better cooling effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 This is a schematic diagram of the overall structure of a reactor for preparing diethyl acetamidomalonate according to a specific embodiment of the present invention; Figure 2 This is a schematic structural diagram of a raw material dropping assembly of a reactor for preparing diethyl acetamidomalonate according to a specific embodiment of the present invention; Figure 3 for Figure 2 Schematic diagram of the back structure of the raw material dripping assembly; Figure 4 for Figure 2 A schematic diagram of the structure of the fixed cylinder of the raw material dropping assembly; Figure 5 It is a structural schematic diagram of a linkage structure of a reaction kettle for preparing diethyl acetamidomalonate according to a specific embodiment of the present invention; Figure 6 This is a schematic structural diagram of a stirring structure of a reactor for preparing diethyl acetamidomalonate according to a specific embodiment of the present invention; Figure 7 This is a schematic structural diagram of an auxiliary cooling component of a reactor for preparing diethyl acetamidomalonate according to a specific embodiment of the present invention; Figure 8 for Figure 7 Schematic diagram of auxiliary cooling components during rapid movement; Fig. 9 for Figure 7 A schematic diagram of the structure of the circular fixed shell of the auxiliary cooling component; Fig.10 for Figure 7 A schematic diagram of the structure of the ice water bin of the auxiliary cooling component; Fig.11 for Figure 1 A front view of the overall structure of the reactor without the linkage device; Fig.12 The present invention is a schematic diagram of a control valve connection structure of a reactor for preparing diethyl acetamidomalonate according to a specific embodiment of the present invention.

[0023] In the figure: Fixed base 1; Kettle body 2, temperature gauge 201; Kettle cover 3, feed pipe 301, pressure gauge 302; Fixed plate frame 4, guide slide 401; Raw material dropping component 5, moving slider 501, rotating disk 502, rocker 503, servo motor 504, fixed tripod 505, fixed cylinder 506, moving piston 507, moving guide rod 508, output hose 509, input pipe 510, stirring cylinder 511, feeding hopper 512, stirring motor 513, rotating rod 514, stirring blade 515, conveying pump 516, conveying pipeline 517, high-level tank 518, dropping tube 519, flow control valve 520, connecting shell 521, flow limiting hole 522, flow meter 523; linkage structure 6, fixed horizontal plate 601, guide rod 602, connecting plate 603, rack 604, connecting rod 605, fixed seat 606, rotating rod 607, gear A608, bevel gear A609, rotating rod 610, gear B611, bevel gear B612; Stirring structure 7, stirring shaft 701, stirring blade 702, gear C703, rotary joint 704; Auxiliary cooling component 8, fixed shell 801, heat conduction roller 802, connecting pipe A803, connecting pipe B804, rotating shaft 805, baffle 806, circular fixed shell 807, clockwork spring 808, ice water bin 809, pump 810, output pipe 811, input pipe 812. DETAILED DESCRIPTION

[0024] In order to enable those skilled in the art to better understand the present application, the present invention will be clearly and completely described below with reference to the technical solutions of specific implementation methods in conjunction with the accompanying drawings. Obviously, the described embodiments are merely exemplary, and the present invention is not limited to this specific implementation method.

[0025] It should be noted that the terms "first", "second", etc. in the specification and claims of the present application and the above-mentioned drawings are used to distinguish similar objects, and are not necessarily used to describe a specific order or sequential order. It should be understood that the data used in this way can be interchanged where appropriate, so that the embodiments of the present application described here. In addition, the terms "including" and "having" and any of their variations are intended to cover non-exclusive inclusions, for example, a process, method, system, product or device comprising a series of steps or units is not necessarily limited to those steps or units clearly listed, but may include other steps or units that are not clearly listed or inherent to these processes, methods, products or devices.

[0026] In the present application, the terms "upper", "lower", "left", "right", "front", "back", "top", "bottom", "inner", "outer", "middle", "vertical", "horizontal", "lateral", "longitudinal" and the like indicate positions or positional relationships based on the positions or positional relationships shown in the drawings. These terms are mainly used to better describe the present application and its embodiments, and are not used to limit the indicated devices, elements or components to have a specific orientation, or to be constructed and operated in a specific orientation.

[0027] In addition, some of the above terms may be used to express other meanings in addition to indicating orientation or positional relationship. For example, the term "on" may also be used to express a certain dependency or connection relationship in some cases. For those of ordinary skill in the art, the specific meanings of these terms in this application can be understood according to specific circumstances.

[0028] In addition, the terms "installed", "set", "provided with", "connected", "connected", and "socketed" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral structure; it can be a mechanical connection, or an electrical connection; it can be a direct connection, or an indirect connection through an intermediate medium, or it can be an internal connection between two devices, elements, or components. For those of ordinary skill in the art, the specific meanings of the above terms in this application can be understood according to specific circumstances.

[0029] Figure 1 , 11 A reaction kettle for preparing diethyl acetamidomalonate according to a specific embodiment of the present invention is shown; Figure 2 , 3 The raw material adding assembly of the reactor is shown; Figure 4 The fixed cylinder of the raw material dropping assembly is shown; Figure 5 The linkage structure of the reactor is shown; Figure 6 The stirring structure is shown; Figure 7 , 8 The auxiliary cooling component of the reactor is shown; Figure 8 ,9 The circular fixed shell and ice water tank of the auxiliary cooling assembly are shown.

[0030] like Figure 1 , 11 As shown, the reaction kettle for the reaction preparation of diethyl acetamidomalonate includes: a kettle body 2, the kettle body 2 is fixedly arranged on the upper surface of a fixed base 1, a kettle cover 3 is fixedly connected to the upper end of the kettle body 2, and the kettle body 2 is used for oximation reaction; a raw material dropping component 5, the raw material dropping component 5 is fixed on the side wall of a fixed plate frame 4, the fixed plate frame 4 is fixedly arranged on the upper surface of the fixed base 1, and the raw material dropping component 5 is used for gradually dropping the raw material solution; a linkage structure 6, the linkage structure 6 is fixedly arranged on the top of the fixed plate frame 4, and the bottom end of the linkage structure 6 is connected to the raw material dropping component 5; a stirring structure 7, the stirring structure 7 is arranged at the kettle cover 3, and the stirring structure 7 is used for automatic rotation and stirring during oximation reaction; an auxiliary cooling component 8, the auxiliary cooling component 8 is fixedly arranged at the bottom end of the stirring structure 7, and the auxiliary cooling component 8 is used for automatic cooling during oximation reaction. Through the above technical scheme, the raw material dropping component 5 can be conveniently used to gradually drop the raw materials into the kettle body 2, so that the reaction can be carried out gradually, avoiding the problem of overly intense reaction. Furthermore, the present application has designed a stirring structure 7, through which the stirring structure 7 can automatically stir and mix during the reaction, so that the reaction is sufficient. At the same time, in conjunction with the setting of the linkage structure 6, the stirring rate can be automatically adjusted according to the rate of dropping the raw materials, without the need for an additional power source, solving the problem that the stirring structure of the ordinary reactor in the prior art has a constant speed, and the reactants are slowly added, which is easy to stir relatively quickly to produce a large amount of foam or stir relatively slowly to cause insufficient reaction. At the same time, the present application has set up an auxiliary cooling component 8, through which the temperature in the oximation reaction process can be cooled and controlled, avoiding dangerous situations caused by excessively high temperatures during the reaction process. At the same time, the cooling rate can be automatically controlled in conjunction with the stirring speed, and the phenomenon of too low temperature of the reactants caused by excessive cooling is avoided, achieving a better cooling effect.

[0031] like Figure 2-4As shown, the raw material dripping assembly 5 includes a moving slider 501, a rotating disk 502, a rocker 503, a servo motor 504, a fixed tripod 505, a fixed cylinder 506, a moving piston 507, a moving guide rod 508, an output hose 509 and an input pipe 510. The fixed plate frame 4 is provided with a guide slot 401, and the moving slider 501 is slidably connected to the guide slot 401. The rotating disk 502 is rotatably connected to the side wall of one side of the fixed plate frame 4, and the rotating disk 502 is rotatably connected to the side wall of the rotating disk 502. One end of the rocker 503, the other end of the rocker 503 is rotatably connected to the side wall of the movable slider 501, and the other side of the fixed plate frame 4 is fixedly connected with a servo motor 504, and the end of the output shaft of the servo motor 504 is fixedly connected to the rotating disk 502. According to the technical solution, the rotating disk 502 can be driven to rotate by the operation of the servo motor 504, so that the rocker 503 can be driven to reciprocate by the rotation of the rotating disk 502, thereby driving the movable slider 501 to reciprocate up and down; The fixed tripod 505 is fixedly arranged on the side wall of the fixed plate frame 4, and a fixed cylinder 506 is fixedly connected to the upper surface of the fixed tripod 505. A movable piston 507 is slidably connected in the inner cavity of the fixed cylinder 506. One end of a movable guide rod 508 is fixedly connected to the upper surface of the movable piston 507. The other end of the movable guide rod 508 passes through the upper wall of the inner cavity of the fixed cylinder 506 and extends outside the wall. The top end of the movable guide rod 508 is fixedly connected to the movable slider 501. The bottom side of the inner cavity of the fixed cylinder 506 is fixedly connected to the movable slider 501. One end of the output hose 509 is fixedly connected to the bottom of the inner cavity of the fixed cylinder 506, and the other end of the output hose 509 extends to one end of the feed pipe 301 and is fixedly connected to the feed pipe 301. The output hose 509 is installed with an output check valve. The bottom side of the inner cavity of the fixed cylinder 506 is fixedly connected with an input pipe 510, and the input check valve is installed on the input pipe 510. According to the technical solution, when the raw material solution needs to be gradually added into the reactor, one end of the input pipe 510 is extended to the raw material solution, and the servo motor 504 can be used to The movable slider 501 is driven to move, thereby driving the movable guide rod 508 to move, and then driving the movable piston 507 to move. The raw material solution can be sucked by moving the movable piston 507 upward. When the movable piston 507 is pressed downward, the raw material solution is transported to the feed pipe 301 through the output hose 509, thereby entering the reactor for reaction. Through the above technical scheme, the gradual addition of raw materials can be achieved, avoiding the problem of excessive reaction caused by adding raw materials at one time. At the same time, the speed of gradual addition can be controlled by controlling the rotation speed of the rotating disk 502 by the servo motor 504. When it is necessary to speed up the input of raw materials, the rotation of the rotating disk 502 can be accelerated by the servo motor 504, and then the movement frequency of the movable slider 501 can be increased, thereby increasing the frequency of raw material addition. When it is necessary to slow down the input of raw materials, conversely, the rotation speed of the rotating disk 502 is reduced, so that the frequency of raw material input can be reduced, and the speed is reduced, thereby realizing the regulation function. It is particularly suitable for use in the oximation reaction in the preparation of diethyl acetamidomalonate.

[0032] like Figure 5As shown, the linkage structure 6 includes a fixed transverse plate 601, a guide rod 602, a connecting plate 603, a rack 604, a connecting rod 605, a fixed seat 606, a rotating rod 607, a gear A608, a bevel gear A609, a rotating rod 610, a gear B611 and a bevel gear B612. The fixed transverse plate 601 is fixedly arranged on the side wall of the fixed plate frame 4. The fixed transverse plate 601 is slidably connected with the guide rod 602. The upper and lower ends of the guide rod 602 are fixedly connected with connecting plates 603. The bottom side of the connecting plate 603 is fixedly connected with one end of the connecting rod 605. The other end of the connecting rod 605 is fixedly connected to the moving slider 501. A rack 604 is fixedly connected between the two connecting plates 603, and the rack 604 passes through the fixed transverse plate 601. The upper surface of the fixed horizontal plate 601 is fixedly connected with a fixed seat 606, and the fixed seat 606 is rotatably connected with a rotating rod 607, one end of the rotating rod 607 is fixedly connected with a gear A608, the gear A608 and the rack 604 are meshed with each other, and the other end of the rotating rod 607 is fixedly connected with a bevel gear A609, and the fixed horizontal plate 601 is rotatably connected with a rotating rod 610, the upper end of the rotating rod 610 is fixedly connected with a bevel gear B612, the bevel gear B612 and the bevel gear A609 are meshed with each other, and the bottom end of the rotating rod 610 is fixedly connected with a gear B611. Through the technical solution, When the movable slider 501 moves, the connecting rod 605 can be driven to move, so that the movement of the connecting rod 605 can drive the guide rod 602 to move, and then drive the rack 604 to move. The movement of the rack 604 can drive the gear A608 to rotate, thereby driving the rotating rod 607 to rotate. The rotation of the rotating rod 607 can drive the bevel gear A609 to rotate, and then drive the bevel gear B612 to rotate. The rotation of the bevel gear B612 can drive the gear B611 to rotate. Through this technical solution, the function of automatically driving the gear B611 to rotate during the gradual dripping of the raw materials can be realized.

[0033] like Figure 6As shown, the stirring structure 7 includes a stirring shaft 701, a stirring blade 702, a gear C703 and a rotary joint 704. The stirring shaft 701 is arranged at the kettle cover 3 and is rotatably connected to the kettle cover 3. The bottom end of the stirring shaft 701 is fixedly connected with the stirring blade 702, and the upper arc wall of the stirring shaft 701 is fixedly connected with the gear C703. The gear C703 and the gear B611 are meshed with each other. Through the technical solution, the rotation of the gear B611 can drive the gear C703 to rotate, and the rotation of the gear C703 can drive the stirring shaft 701 to rotate, and then drive the stirring blade 702 to rotate, so that the raw material solution in the reactor can be stirred to make it fully reacted. At the same time, when the speed of adding the raw material changes, the stirring speed will automatically make a corresponding adjustment. When the speed of adding the raw material solution changes, the stirring speed will automatically make a corresponding adjustment. When the rate increases, the rotation speed of the gear B611 will also increase, so that the rotation speed of the stirring shaft 701 increases, and then the stirring speed can be increased with the addition of raw materials, so that the raw materials can be fully mixed. When the rate of adding raw materials decreases, the stirring speed will also be automatically reduced, avoiding the phenomenon of generating a large amount of foam due to long-term rapid stirring. The problem that the ordinary stirring structure in the prior art has a fixed stirring speed and the raw material addition speed is relatively fast relative to the stirring speed, which is prone to uneven mixing and insufficient reaction, and the problem that the raw material addition speed is relatively slow relative to the stirring speed, and a large amount of foam is generated during long-term rapid stirring, the stirring structure of the present application can automatically adapt to the change according to the speed of raw material addition, and does not require an additional power source, and is particularly suitable for use in the oximation reaction in the preparation of diethyl acetamidomalonate; The stirring shaft 701 is provided with an inner cavity, and a rotating joint 704 is fixedly connected to the upper end of the stirring shaft 701 .

[0034] As a further preferred embodiment of the technical solution, Figure 7-10 As shown, the auxiliary cooling component 8 includes a fixed shell 801, a heat-conducting roller 802, a connecting pipe A803, a connecting pipe B804, a rotating shaft 805, a baffle 806, a circular fixed shell 807, a spring 808, an ice water bin 809 and a pump 810. The fixed shell 801 is fixedly arranged at the arc wall of the stirring shaft 701. A plurality of heat-conducting rollers 802 are fixedly arranged in the inner cavity of the fixed shell 801. A connecting pipe A803 is fixedly connected between the plurality of heat-conducting rollers 802. One end of a connecting pipe B804 is fixedly connected in the inner cavity of the stirring shaft 701. The other end of the connecting pipe B804 is fixedly connected to the heat-conducting roller 802. Ice water is arranged in the inner cavity of the ice water bin 809, and a pump 810 is fixedly connected to the upper surface of the ice water bin 809, and the input end of the pump 810 is fixedly connected to one end of an input pipe 812, and the other end of the input pipe 812 extends into the ice water, and the output end of the pump 810 is fixedly connected to one end of an output pipe 811, and the other end of the output pipe 811 is connected to the rotary joint 704. Through the technical solution, the ice water can be transported to the inner cavity of the stirring shaft 701 through the operation of the pump 810, and then transported to the heat-conducting roller 802 and the connecting pipe A803 through the connecting pipe B804, and then through the setting of the heat-conducting roller 802, the raw material solution in the reactor can be cooled, thereby avoiding the dangerous situation caused by the rapid temperature increase caused by the release of a large amount of heat during the oximation reaction, and realizing the automatic cooling function during the stirring process; The openings on both sides of the fixed shell 801 are rotatably connected with a rotating shaft 805, and the arc-shaped wall of the rotating shaft 805 is fixedly connected with a baffle 806. The upper surface of the fixed shell 801 is fixedly connected with a circular fixed shell 807, and one end of the rotating shaft 805 extends into the inner cavity of the circular fixed shell 807, and one end of a spring 808 is fixedly connected to the inner cavity of the circular fixed shell 807, and the other end of the spring 808 is fixedly connected to the rotating shaft 805. Through the technical solution, the baffle 806 is set to shield and block the raw material solution. During the rotation of the stirring shaft 701, when the rotation speed of the stirring shaft 701 is accelerated, the moving speed of the fixed shell 801 will be accelerated. As the speed of the fixed shell 801 is accelerated, the force of the solution pushing the baffle 806 will increase, so that The baffle 806 is flipped to open the opening, so that the raw material solution can quickly contact the heat-conducting roller 802, thereby accelerating the cooling speed. On the contrary, when the rotation speed of the stirring shaft 701 decreases, the speed of the fixed shell 801 is slow, which will reduce the force of the solution to push the baffle 806, so that the baffle 806 is in a closed state, and the solution cannot quickly flow in the inner cavity of the fixed shell 801, thereby slowing down the cooling speed. From the above description, it can be seen that the auxiliary cooling component 8 of the present application can change synchronously when the raw material addition speed changes. On the one hand, it avoids the high temperature danger caused by heating. On the other hand, after the raw material gradually stops adding, the cooling speed is slowed down, avoiding the problem of excessive temperature, reduced reaction speed and incomplete reaction caused by excessive cooling, realizing the function of automatic adjustment, and does not require an additional power source, which is easy to use.

[0035] Fig.11 for Figure 1 A front view of the overall structure of the reactor without the linkage device; Fig.12 Figure 1 is a schematic diagram of the control valve connection structure. Figure 7 , 8As shown in Figures 11 and 12, the raw material dropping component 5 includes a mixing drum 511, a feed hopper 512, a stirring motor 513, a rotating rod 514, a stirring blade 515, a delivery pump 516, a delivery pipeline 517, a high-level tank 518, a dripping pipe 519, a flow control valve 520, a connecting shell 521, a flow limiting hole 522 and a flow meter 523. The mixing drum 511 is fixedly arranged on the upper surface of the fixed base 1, and the feeding hopper 512 is fixedly connected to the upper side of the inner cavity of the mixing drum 511. The stirring motor 513 is fixedly connected to the upper surface of the mixing drum 511. The output end of the stirring motor 513 is fixedly connected to one end of the rotating rod 514. The other end of the rotating rod 514 extends into the inner cavity of the mixing drum 511. A stirring piece 515, a delivery pump 516 is fixedly connected to the side of the stirring drum 511, an input end of the delivery pump 516 extends into the inner cavity of the stirring drum 511, an output end of the delivery pump 516 is fixedly connected to one end of a delivery pipe 517, and the other end of the delivery pipe 517 extends into the interior of the kettle cover 3 and is fixedly connected to the kettle cover 3. According to the technical solution, water required for the oximation reaction is put into the inner cavity of the stirring drum 511, and then sodium nitrite is put into the interior of the stirring drum 511. The stirring piece 515 can be driven to rotate by the operation of the stirring motor 513 to mix and form a sodium nitrite solution. The sodium nitrite solution can be put into the inner cavity of the kettle body 2 by the operation of the delivery pump 516, and then diethyl malonate is put into the reactor; like Fig.11 , 12 As shown, the high-level tank 518 is fixedly arranged at the upper end position of the fixed plate frame 4, the inner cavity of the high-level tank 518 is filled with glacial acetic acid, one end of the dripping tube 519 is fixedly connected to the bottom end of the inner cavity of the high-level tank 518, the other end of the dripping tube 519 extends into the inner cavity of the kettle body 2, one end of the dripping tube 519 is fixedly connected to a connecting shell 521, a plurality of flow limiting holes 522 are arranged at the bottom wall of the inner cavity of the connecting shell 521, a flow control valve 520 is installed on the dripping tube 519, and a flow meter 523 is installed on the dripping tube 519. Through the technical solution, the glacial acetic acid to be dripped is transported to the inner cavity of the kettle body 2 through the dripping tube 519 by gravity, and the addition rate can be controlled by the flow control valve 520, so as to avoid the violent reaction caused by adding too fast at one time, and the flow limiting hole 522 is arranged, so that the acetic acid can be evenly dripped into the reactor.

[0036] In actual preparation, four reactors are usually used in parallel for oximation reaction. As a feeding method, it is preferred to design a sodium nitrite dissolving kettle separately to dissolve sodium nitrite, design a barrel structure separately to contain diethyl malonate and process water, and use a diaphragm pump to pump diethyl malonate into the dissolving kettle.

[0037] In a preferred embodiment, the oximation synthesis feeding method comprises the following steps: 1. Use a diaphragm pump to input 800kg barrels of process water into the sodium nitrite dissolving kettle; 2. Open the dissolving kettle cover and put 200kg sodium nitrite into the kettle; 3. Use a diaphragm pump to input 400 kg of diethyl malonate into the dissolving kettle; 4. Start stirring the dissolving kettle, stir for 30 minutes, then open the bottom valve of the dissolving kettle and put the materials in the dissolving kettle into the designated oximation reactor; 5. Pump 184 kg of glacial acetic acid into the high-level tank and add it dropwise.

[0038] According to the present invention, since the raw material dropping component can conveniently drop the raw materials into the kettle body step by step, so that the reaction can proceed step by step, the problem of overly intense reaction can be effectively avoided. Furthermore, the present application has designed a special stirring structure, through which the stirring structure can automatically stir and mix during the reaction to ensure sufficient reaction. At the same time, with the setting of the linkage structure, the stirring rate can be automatically adjusted according to the rate of dropping the raw materials, without the need for an additional power source. In a preferred embodiment, the feeding method can also be designed separately, so that the oximation reaction can be further safely controlled.

[0039] In summary, the present invention has been described in detail. However, those skilled in the art will appreciate that the present invention can be modified and altered in various ways. For example, the present invention is described with the input ratio of sodium nitrite: process water: diethyl malonate: glacial acetic acid being 200kg: 800kg: 400kg: 184kg. However, corresponding changes can actually be made, and it is possible to increase or reduce some weight simultaneously. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of this application shall fall within the protection scope of the present invention, and the protection scope of the present invention is defined by the attached claims.

Claims

1. A reactor for the reaction preparation of diethyl acetamidomalonate, characterized in that: The reactor for preparing diethyl acetamidomalonate by reaction comprises: A kettle body (2), the kettle body (2) being fixedly arranged on the upper surface of the fixed base (1), a kettle cover (3) being fixedly connected to the upper end of the kettle body (2), and the kettle body (2) being used for performing an oximation reaction; A raw material dripping assembly (5), the raw material dripping assembly (5) being fixed to a side wall of a fixed plate frame (4), the fixed plate frame (4) being fixedly arranged on an upper surface of a fixed base (1), the raw material dripping assembly (5) being used for gradually dripping a raw material solution; A linkage structure (6), wherein the linkage structure (6) is fixedly arranged on the top of the fixed plate frame (4), and the bottom end of the linkage structure (6) is connected to the raw material dripping assembly (5); A stirring structure (7), wherein the stirring structure (7) is arranged on the kettle cover (3), and the stirring structure (7) is used to automatically rotate and stir during the oximation reaction; An auxiliary cooling component (8) is fixedly arranged at the bottom end of the stirring structure (7), and the auxiliary cooling component (8) is used to automatically cool down during the oximation reaction.

2. The reactor for the preparation of diethyl acetamidomalonate according to claim 1, characterized in that: The raw material dropping assembly (5) comprises a movable slider (501), a rotating disk (502), a rocker (503), a servo motor (504), a fixed foot frame (505), a fixed cylinder (506), a movable piston (507), a movable guide rod (508), an output hose (509) and an input pipe (510). A guide slot (401) is provided at the fixed plate frame (4), and the movable slider (501) is slidably connected to the guide slot (401). The rotating disk (502) is rotatably connected to a side wall of one side of the fixed plate frame (4), and one end of the rocker (503) is rotatably connected to the side wall of the rotating disk (502). The other end of the rocker (503) is rotatably connected to the side wall of the movable slider (501). The servo motor (504) is fixedly connected to the other side of the fixed plate frame (4), and the output shaft end of the servo motor (504) is fixedly connected to the rotating disk (502).

3. The reactor for the reaction preparation of diethyl acetamidomalonate according to claim 2, characterized in that: The fixed bracket (505) is fixedly arranged on the side wall of the fixed plate frame (4); a fixed cylinder (506) is fixedly connected to the upper surface of the fixed bracket (505); a movable piston (507) is slidably connected in the inner cavity of the fixed cylinder (506); one end of a movable guide rod (508) is fixedly connected to the upper surface of the movable piston (507); the other end of the movable guide rod (508) penetrates the upper wall of the inner cavity of the fixed cylinder (506) and extends outside the wall; The top end is fixedly connected to the movable slider (501); one end of an output hose (509) is fixedly connected to the bottom side of the inner cavity of the fixed cylinder (506); the other end of the output hose (509) extends to one end of the feed pipe (301) and is fixedly connected to the feed pipe (301); an output check valve is installed on the output hose (509); an input pipe (510) is fixedly connected to the bottom side of the inner cavity of the fixed cylinder (506); and an input check valve is installed on the input pipe (510).

4. The reactor for preparing diethyl acetamidomalonate according to claim 1, characterized in that: The linkage structure (6) comprises a fixed transverse plate (601), a guide rod (602), a connecting plate (603), a rack (604), a connecting rod (605), a fixed seat (606), a rotating rod (607), a gear A (608), a bevel gear A (609), a rotating rod (610), a gear B (611) and a bevel gear B (612); the fixed transverse plate (601) is fixedly arranged on a side wall of the fixed plate frame (4); the fixed transverse plate (601) is slidably connected to the guide rod (602); the upper and lower ends of the guide rod (602) are fixedly connected to the connecting plates (603); one end of the connecting rod (605) is fixedly connected to the bottom connecting plate (603); the other end of the connecting rod (605) is fixedly connected to the movable slider (501); a rack (604) is fixedly connected between the two connecting plates (603); and the rack (604) passes through the fixed transverse plate (601).

5. The reactor for preparing diethyl acetamidomalonate by reaction according to claim 4, characterized in that: A fixed seat (606) is fixedly connected to the upper surface of the fixed horizontal plate (601), a rotating rod (607) is rotatably connected to the fixed seat (606), a gear A (608) is fixedly connected to one end of the rotating rod (607), the gear A (608) and the rack (604) are meshed with each other, a bevel gear A (609) is fixedly connected to the other end of the rotating rod (607), a rotating rod (610) is rotatably connected to the fixed horizontal plate (601), a bevel gear B (612) is fixedly connected to the upper end of the rotating rod (610), the bevel gear B (612) and the bevel gear A (609) are meshed with each other, and a gear B (611) is fixedly connected to the bottom end of the rotating rod (610).

6. The reactor for preparing diethyl acetamidomalonate according to claim 1, characterized in that: The stirring structure (7) comprises a stirring shaft (701), a stirring blade (702), a gear C (703) and a rotary joint (704); the stirring shaft (701) is arranged at the kettle cover (3) and is rotatably connected to the kettle cover (3); the stirring blade (702) is fixedly connected to the bottom end of the stirring shaft (701); the gear C (703) is fixedly connected to the arc-shaped wall at the upper end of the stirring shaft (701); and the gear C (703) and the gear B (611) are meshed with each other.

7. The reactor for preparing diethyl acetamidomalonate according to claim 6, characterized in that: An inner cavity is provided inside the stirring shaft (701), and a rotating joint (704) is fixedly connected to the upper end of the stirring shaft (701).

8. The reactor for preparing diethyl acetamidomalonate according to claim 1, characterized in that: The auxiliary cooling component (8) comprises a fixed shell (801), a heat-conducting roller (802), a connecting pipe A (803), a connecting pipe B (804), a rotating shaft (805), a baffle (806), a circular fixed shell (807), a spring (808), an ice water bin (809) and a pump (810); the fixed shell (801) is fixedly arranged on the arc-shaped wall of the stirring shaft (701); a plurality of heat-conducting rollers (802) are fixedly arranged in the inner cavity of the fixed shell (801); a connecting pipe A (803) is fixedly connected between the plurality of heat-conducting rollers (802); one end of a connecting pipe B (804) is fixedly connected in the inner cavity of the stirring shaft (701); and the other end of the connecting pipe B (804) is fixedly connected to the heat-conducting roller (802).

9. The reactor for the reaction preparation of diethyl acetamidomalonate according to claim 8, characterized in that: Ice water is arranged in the inner cavity of the ice water bin (809); a pump (810) is fixedly connected to the upper surface of the ice water bin (809); an input end of the pump (810) is fixedly connected to one end of an input pipe (812); the other end of the input pipe (812) extends into the ice water; an output end of the pump (810) is fixedly connected to one end of an output pipe (811); the other end of the output pipe (811) is connected to a rotary joint (704).

10. The reactor for preparing diethyl acetamidomalonate according to claim 8, characterized in that: The openings on both sides of the fixed shell (801) are rotatably connected to a rotating shaft (805), a baffle (806) is fixedly connected to the arc-shaped wall of the rotating shaft (805), a circular fixed shell (807) is fixedly connected to the upper surface of the fixed shell (801), one end of the rotating shaft (805) extends into the inner cavity of the circular fixed shell (807), one end of a clockwork spring (808) is fixedly connected to the inner cavity of the circular fixed shell (807), and the other end of the clockwork spring (808) is fixedly connected to the rotating shaft (805).

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