Malonic acid mono-p-nitrobenzyl ester heat preservation preparation device

Abstract

The present invention discloses a malonic acid mono-p-nitrobenzyl ester thermal insulation preparation apparatus, and belongs to the field of malonic acid mono-p-nitrobenzyl ester synthesis, the malonic acid mono-p-nitrobenzyl ester thermal insulation preparation apparatus comprises a shell and a side plate fixedly connected to one side of the shell, the upper end of the shell is provided with three groups of feed ports I, and the interior of the shell is connected with a pre-dissolving and mixing unit; the pre-dissolving and mixing unit comprises two raw material dissolving and mixing assemblies symmetrically connected to the interior of the shell and a catalytic dissolving and mixing assembly connected to the interior of the shell, and a final dissolving and mixing unit is further connected to the interior of the shell; the method comprises the following steps: pre-dissolving and mixing malonic acid diester and a solvent and p-nitrobenzyl alcohol and a solvent through two raw material dissolving and mixing assemblies respectively, pre-dissolving and mixing a catalyst and the solvent through a catalytic dissolving and mixing assembly, fully dissolving reactants in respective solvents respectively, and then mixing to obtain a mixed solution; therefore, the reactant precipitation or precipitation phenomenon caused by the solubility difference can be avoided, and each reactant is ensured to reach a higher concentration in the solvent most suitable for dissolving the reactant.

Description

Technical Field

[0001] The invention relates to the field of synthesis of mono-p-nitrobenzyl malonate, and more specifically to a thermal insulation preparation device for mono-p-nitrobenzyl malonate. Background Art

[0002] Mono-p-nitrobenzyl malonate (also known as nitrobenzyl malonate) is a common organic chemical intermediate, widely used in drug synthesis and the production of fine chemicals. At present, the most commonly used synthesis method for large-scale production of mono-p-nitrobenzyl malonate is usually the ester exchange method, mainly because of its high reaction efficiency, low by-product generation and easy operation.

[0003] The ester exchange method for preparing mono-p-nitrobenzyl malonate is based on p-nitrobenzyl alcohol and diester of malonate as raw materials. The diester of malonate and p-nitrobenzyl alcohol are dissolved in a solvent under the catalysis of a catalyst, and then a series of post-treatments such as washing and purification are performed to obtain mono-p-nitrobenzyl malonate. However, in the mixed dissolution process of the ester exchange reaction, the solubility of different reactants (such as diester of malonate and p-nitrobenzyl alcohol) and the catalyst in the solvent may be different, which will result in the reactants failing to dissolve completely, affecting the reaction rate and product yield. Summary of the invention

[0004] In view of the problems existing in the prior art, the object of the present invention is to provide a thermal insulation preparation device for mono-p-nitrobenzyl malonate.

[0005] To solve the above problems, the present invention adopts the following technical solutions.

[0006] A thermal insulation preparation device for mono-p-nitrobenzyl malonate, comprising a shell, a side plate fixed to one side of the shell, and three groups of feed ports opened at the upper end of the shell; a pre-mixing unit and a final mixing unit are connected inside the shell; the pre-mixing unit comprises two raw material mixing components symmetrically connected inside the shell, and a catalytic mixing component connected inside the shell; the final mixing unit is connected to the two raw material mixing components and the catalytic mixing component through a feeding part; The raw material dissolving and mixing assembly comprises a container 1 fixedly connected to the inner wall of the shell, a stator 1 fixedly connected to the inner wall of the shell and located inside the container 1, a motor 1 fixedly connected to the outer surface of the upper end of the shell, and a rotor 1 having one end fixedly connected to the output shaft of the motor 1 and the other end rotatably connected to the stator 1; The catalytic dissolving and mixing assembly comprises a container 2 fixedly connected to the inner wall of the shell and located between the two containers 1, a stator 2 fixedly connected to the inner wall of the shell and located inside the container 2, a motor 2 fixedly connected to the outer surface of the upper end of the shell, and a rotor 2 having one end fixedly connected to the output shaft of the motor 2 and the other end rotatably connected to the stator 2; The feeding part includes two mixing parts symmetrically fixed to the upper end of the support plate, a pump body 1 fixed to the lower end of the two containers and connected to the output end of the first container, three pump bodies 2 fixed to the lower end of the second container and connected to the three output ends at the bottom of the second container, two groups of support plates fixed to the inner wall of the shell and the side plate, and two rotary joints 1 respectively connected to the two groups of support plates, and the mixing part includes a feeding part, a throat and a diffusion part, wherein the output ends of two of the pump bodies 2 are respectively connected to the two throats, the output ends of two of the pump bodies 1 are respectively connected to the input ends of two rotary joints 1, and the output end of the other pump body 2 is connected to the input end of the rotary joint 2.

[0007] Furthermore, a support plate is fixedly connected to the inner wall of the shell, and two feed ports 2 connected to the feeding part are symmetrically provided in the support plate. The final mixing unit includes a container 3 fixedly connected to the lower end of the support plate, a guide rod fixedly connected to the inner bottom wall of the container 3, a rod body movably sleeved on the outside of the guide rod, a movable seat movably connected to the inside of the shell, a rotary joint 2 fixedly connected to the upper end of the movable seat and connected to the feeding part, a hollow cavity provided in the inside of the rod body and a discharge port provided on the outer surface of the rod body and connected to the hollow cavity, a stator 3 fixedly connected to the lower end of the movable seat and penetrating the support plate and extending into the inside of the container 3, a shear sheet fixedly connected to the outside of the rod body and located in the stator 3, a driving part connected to the inside of the movable seat for driving the rod body to rotate, and the inner tube of the rotary joint 2 is inserted into the hollow cavity and fixedly connected to the inner wall of the hollow cavity.

[0008] Furthermore, the other end of the rod body is rotatably connected to the inside of the movable seat, and the driving part includes a motor five fixed to the upper end of the movable seat, a gear three rotatably connected to the inside of the movable seat and fixed to the output shaft of the motor five, and a gear four rotatably connected to the inside of the movable seat and fixed to the outer surface of the rod body, and gear three is meshed with gear four.

[0009] Furthermore, a heating jacket is fixedly connected to the outer surface of the container.

[0010] Furthermore, a spiral guide flange is integrally formed inside the throat, the upper ends of the two feed parts are rotatably connected to gear two, the upper ends of the two groups of support plates are respectively fixed with two motors three, and the lower ends of the two groups of support plates are respectively rotatably connected to two gears one meshing with gear two, the output shaft of motor three passes through the support plate and is connected to gear one, and gear two is fixedly sleeved on the outside of the inner tube of rotary joint one.

[0011] Furthermore, the outer surface of one side of the shell and the outer surface of one side of the side plate are both connected to a lifting part, and the lifting part includes two groups of fixed plates respectively fixed to one side of the shell and one side of the side plate, a motor four rotatably connected to a screw rod and fixed to the outer surface of one side of the side plate with one group of fixed plates, and a guide rod fixed to the other group of fixed plates, and the output shaft of motor four passes through the fixed plate and is connected to the screw rod, movable grooves are opened inside the shell and the side plate, and two ends of the movable seat extend outward through the movable grooves, the extended end on one side of the movable seat is screwed to the outside of the screw rod and the extended end on the other side is movably sleeved on the outside of the guide rod.

[0012] Furthermore, a circulating defoaming unit is also connected to the inside of the shell, and the circulating defoaming unit includes two positioning plates respectively fixed to the inner wall of the shell and the inner wall of the side plate, a box body located between the two positioning plates and fixed to the two positioning plates on both sides, a pump body four and a pump body three respectively fixed to the upper end and one side of the box body, a one-way exhaust valve connected to the upper end of the box body, an ultrasonic generating part fixed to the lower end of the box body, and the input end of the pump body three is connected to the container three and the output end is connected to the box body, and the input end of the pump body four is connected to the box body and the output end is connected to the container three.

[0013] Furthermore, a conical material discharge tray is fixedly connected to the interior of the container, and a hollow groove is opened in the middle of the conical material discharge tray. The rotor is located in the hollow groove, and the gap between the inner wall of the hollow groove and the outside of the rotor is used for material discharge. A plurality of material discharge rods are fixedly connected to the outside of the rotor, and the lower ends of the material discharge rods are in contact with the upper surface of the conical material discharge tray.

[0014] Furthermore, a plurality of material distribution rods are fixedly connected to the outside of the rotor, and the plurality of material distribution rods are located below the conical material discharge tray.

[0015] Compared with the prior art, the present invention has the following beneficial effects: (1) This scheme is provided with a pre-mixing unit, which pre-mixes the malonic acid diester and the solvent and the p-nitrobenzyl alcohol and the solvent respectively through two raw material mixing components, and then pre-mixes the catalyst and the solvent through a catalytic mixing component. After the reactants are fully dissolved in their respective solvents, they are mixed again. This can avoid the precipitation or precipitation of reactants due to solubility differences, ensure that each reactant reaches a higher concentration in the solvent that is most suitable for its dissolution, optimize the solvent system, avoid the situation where the reaction efficiency is affected by incomplete dissolution, and avoid the problem of uneven concentration caused by incomplete dissolution, thereby improving the uniformity of the reaction. This is very helpful in increasing the reaction rate, avoiding local excess or insufficient reactants, and improving the product yield.

[0016] (2) This scheme is provided with a feeding section, through which a part of the catalyst mixture can be pumped into the mixing section through the pump body 2 and efficiently contact and preliminarily react with the malonic acid diester mixture and the p-nitrobenzyl alcohol mixture in a short time, so that the catalyst can be fully dispersed at an early stage, avoiding catalyst agglomeration or precipitation, and increasing the contact area between the reactant and the catalyst. Since the catalyst and the reactant have been preliminarily mixed in the mixing section before entering the main agitator, the reactant has a good catalyst distribution when entering the agitator, which helps to accelerate the start of the reaction and shorten the mixing time. Compared with the traditional catalyst and reactant that start mixing in the agitator, this pre-mixing step can reduce the start time of the reaction and ensure faster entry into the reaction state. By adding the catalyst in two times (preliminary mixing with the reactant first, and then adding the remaining part), more precise catalyst control can be achieved. The amount of catalyst introduced for the first time is small, which can avoid premature overreaction of the catalyst or excessive local concentration, and control the initial rate of the reaction. The remaining catalyst can be evenly distributed in the main agitator to ensure that the catalyst concentration is appropriate during the reaction and optimize the continuity and yield of the reaction.

[0017] (3) This scheme is provided with a lifting part. By making the movable seat, shear plate and stator move up and down, the uniform distribution of solvent and reactants in the reaction system can be effectively promoted. The up and down movement can effectively break the hierarchical structure of the solution, enhance the diffusion rate between solute molecules and solvent molecules, ensure that the reactants and catalysts can contact quickly and evenly, and at the same time continuously break the original flow field structure and promote the turbulent effect inside the fluid. This helps to mix materials more quickly and evenly, avoid liquid stratification or dead zone formation, improve the fluidity and uniformity of the entire reaction system, and can continuously disturb the fluid in the system to avoid the catalyst from agglomerating in the low shear area, ensuring that the catalyst is continuously in an active reaction state. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a schematic diagram of the overall structure of the present invention; Figure 2 It is a schematic diagram of the internal structure of the housing of the present invention; Figure 3 It is a schematic diagram of the structure of the pre-mixing unit of the present invention; Figure 4 It is a schematic diagram of the structure of the material distribution rod and the material moving rod of the present invention; Figure 5 It is a schematic structural diagram of the feeding part of the present invention; Figure 6 is a cross-sectional view of a mixing portion of the present invention; Figure 7 It is a schematic diagram of the final dissolving and mixing unit structure of the present invention; Figure 8 It is a schematic diagram of the structure of the driving part of the present invention; Fig. 9 It is a schematic diagram of the structure of the circulating material defoaming unit of the present invention.

[0019] Description of the numbers in the figure: 1. Shell; 11. Support plate; 2. Side plate; 3. Feed port 1; 4. Pre-mixing unit; 41. Container 1; 411. Motor 1; 412. Rotor 1; 413. Stator 1; 414. Distributor rod; 415. Conical feed tray; 416. Distributor rod; 42. Container 2; 421. Motor 2; 422. Rotor 2; 423. Stator 2; 5. Feeding section; 51. Pump body 1; 52. Pump body 2; 53. Mixing section; 531. Diffuser; 532. Throat; 533. Feeding section; 534. Spiral guide flange; 54. Support plate; 55. Motor 3; 56. Gear 1; 57. Gear 2; 58. Rotary joint one; 6. Final mixing unit; 61. Container three; 611. Guide rod; 62. Heating sleeve; 63. Feed port two; 64. Lifting part; 641. Fixed plate; 642. Screw rod; 643. Motor four; 65. Movable seat; 66. Driving part; 661. Motor five; 662. Gear three; 663. Gear four; 67. Rotary joint two; 68. Rod body; 681. Discharge port; 682. Shear piece; 69. Stator three; 7. Circulating material defoaming unit; 71. Box body; 72. Positioning plate; 73. Pump body three; 74. Pump body four; 75. Ultrasonic generating part; 76. One-way exhaust valve. DETAILED DESCRIPTION

[0020] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention; it is obvious that the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments, and all other embodiments obtained by ordinary technicians in this field based on the embodiments of the present invention without making creative work are within the scope of protection of the present invention.

[0021] See also Figures 1 to 9 A thermal insulation preparation device for mono-p-nitrobenzyl malonate, comprising a shell 1, a side plate 2 fixed to one side of the shell 1, and three groups of feed ports 3 opened at the upper end of the shell 1, wherein a pre-mixing unit 4 and a final mixing unit 6 are connected inside the shell 1, wherein the pre-mixing unit 4 comprises two raw material mixing components symmetrically connected inside the shell 1, and a catalytic mixing component connected inside the shell 1, and an input end of the final mixing unit 6 is connected to the output ends of the two raw material mixing components and the output end of the catalytic mixing component through a feeding portion 5; The raw material dissolving and mixing assembly includes a container 41 fixedly connected to the inner wall of the shell 1, a stator 413 fixedly connected to the inner wall of the shell 1 and located inside the container 41, a motor 411 fixedly connected to the outer surface of the upper end of the shell 1, and a rotor 412 having one end fixedly connected to the output shaft of the motor 411 and the other end rotatably connected to the stator 413; The catalytic dissolving and mixing assembly includes a container 2 42 fixedly connected to the inner wall of the shell 1 and located between two containers 1 41, a stator 2 423 fixedly connected to the inner wall of the shell 1 and located inside the container 2 42, a motor 2 421 fixedly connected to the outer surface of the upper end of the shell 1, and a rotor 2 422, one end of which is fixedly connected to the output shaft of the motor 2 421 and the other end is rotatably connected to the stator 2 423. A conical material discharge tray 415 is also fixedly connected to the inside of the container 1 41, and a hollow groove is opened in the middle of the conical material discharge tray 415. The rotor 1 412 is located in the hollow groove and the gap between the inner wall of the hollow groove and the outside of the rotor 1 412 is used for material discharge. A plurality of material removal rods 416 are fixedly connected to the outside of the rotor 1 412, and the lower end of the material removal rod 416 is in contact with the upper surface of the conical material discharge tray 415. A plurality of material distribution rods 414 are fixedly connected to the outside of the rotor 1 412, and the plurality of material distribution rods 414 are located below the conical material discharge tray 415.

[0022] The inner wall of the shell 1 is fixedly connected to a support plate 11, and two feed ports 63 connected to the feeding part 5 are symmetrically opened in the support plate 11. The final dissolving and mixing unit 6 includes a container 3 61 fixedly connected to the lower end of the support plate 11, a guide rod 611 fixedly connected to the inner bottom wall of the container 3 61, a rod body 68 movably sleeved on the outside of the guide rod 611, a movable seat 65 movably connected to the inside of the shell 1, a rotary joint 67 fixedly connected to the upper end of the movable seat 65 and connected to the feeding part 5, and an opening A hollow cavity is arranged inside the rod body 68, a discharge port 681 is opened on the outer surface of the rod body 68 and communicated with the hollow cavity, a stator three 69 is fixedly connected to the lower end of the movable seat 65 and passes through the support plate 11 to extend into the interior of the container three 61, a shear piece 682 is fixedly connected to the outside of the rod body 68 and located inside the stator three 69, a driving part 66 is connected to the inside of the movable seat 65 for driving the rod body 68 to rotate, and the inner tube of the rotary joint two 67 is inserted into the hollow cavity and fixedly connected to the inner wall of the hollow cavity.

[0023] The other end of the rod body 68 is rotatably connected to the inside of the movable seat 65, and the driving part 66 includes a motor 5 661 fixed to the upper end of the movable seat 65, a gear 3 662 rotatably connected to the inside of the movable seat 65 and fixed to the output shaft of the motor 5 661, and a gear 4 663 rotatably connected to the inside of the movable seat 65 and fixed to the outer surface of the rod body 68, and the gear 3 662 is meshed with the gear 4 663. A heating sleeve 62 is fixed to the outer surface of the container 3 61.

[0024] By adopting the above technical scheme, malonic acid diester and p-nitrobenzyl alcohol are added to two containers 1 41 respectively, a catalyst is added to container 2 42, and then solvent is added to two containers 1 41 and container 2 42. When the raw materials enter the two containers 1 41, they first fall on the conical feeding tray 415, and the motor 1 411 and the motor 2 421 are controlled to work to drive the rotor 1 412 and the rotor 2 422 to rotate respectively (the outer surfaces of the rotor 1 412 and the rotor 2 422 are provided with blades, and the stator 1 413, the stator 2 423 and the stator 3 69 are all composed of a layer of ring with holes The rotor 1 412 is mainly composed of a stator 416 and a stator 414, which mainly guide and further disperse the material. It belongs to the common structural design of the high shear agitator in the prior art and will not be described here. The rotation of the rotor 1 412 drives the material-pickup rod 416 and the material-distribution rod 414 to rotate. The rotation of the material-pickup rod 416 can drive the raw materials on the conical material-discharging tray 415 to move, so that the raw materials fall evenly from between the conical material-discharging tray 415 and the rotor 1 412. The material-distribution rod 414 can break up the fallen raw materials so that the raw materials are dispersed on the surface of the solvent. The rotation of the rotor 1 412 and the rotor 2 422 is respectively connected with the stator 1 416 and the stator 2 414. 3 and stator two 423 cooperate with high speed rotation to generate strong shear force, so that the malonic acid diester and solvent, the nitrobenzyl alcohol and solvent, and the catalyst and solvent are pre-mixed and dissolved to obtain the malonic acid diester solution, the nitrobenzyl alcohol solution, and the catalyst solution respectively, and then the malonic acid diester solution, the nitrobenzyl alcohol solution, and the catalyst solution are fed into the container three 61 through the feeding part 5, and the motor five 661 drives the rod body 68 and the shearing piece 682 to rotate, and the shearing piece 682 cooperates with the stator three 69 to rotate at high speed to generate strong shear force, and is fed into the container three 61 by the feeding part 5. The catalyst solution in the rotary joint 2 67 is discharged from the discharge port 681, and is quickly mixed and dissolved with the sheared solution in the container 3 61. After the reactants are fully dissolved in their respective solvents, the obtained multiple solutions are mixed. This can avoid the precipitation or precipitation of reactants due to solubility differences, ensure that each reactant reaches a higher concentration in the most suitable solvent for its dissolution, optimize the solvent system, avoid the situation where the reaction efficiency is affected by incomplete dissolution, and avoid the problem of uneven concentration caused by incomplete dissolution, thereby improving the uniformity of the reaction. This is very helpful for increasing the reaction rate, avoiding local excess or insufficient reactants, and improving the product yield.

[0025] like Figure 5 and Figure 6As shown, the feeding portion 5 includes two mixing portions 53 symmetrically fixed to the upper end of the support plate 11, a pump body 51 fixed to the lower ends of two containers 41 and connected to the output end of the container 41, three pump bodies 52 fixed to the lower end of the container 42 and connected to the three output ends at the bottom of the container 42, two groups of support plates 54 fixed to the inner walls of the shell 1 and the side plate 2, and two rotary joints 58 respectively connected to the two groups of support plates 54, and the mixing portion 53 includes a feeding portion 533, a throat 532 and a diffusion portion 531, wherein the output ends of the two pump bodies 52 are respectively connected to the two throats 532, the output ends of the two pump bodies 51 are respectively connected to the input ends of the two rotary joints 58, and the output end of the other pump body 52 is connected to the input end of the rotary joint 67.

[0026] A spiral guide flange 534 is integrally formed inside the throat portion 532, and the upper ends of the two feeding portions 533 are rotatably connected to gear two 57, and the upper ends of the two groups of support plates 54 are respectively fixedly connected to two motors three 55, and the lower ends of the two groups of support plates 54 are respectively rotatably connected to two gears one 56 meshing with gear two 57, and the output shaft of motor three 55 passes through the support plate 54 and is connected to gear one 56, and gear two 57 is fixedly sleeved on the outside of the inner tube of the rotary joint one 58.

[0027] By adopting the above technical solution, the two pump bodies 1 51 can respectively pump the diester malonate solution and the p-nitrobenzyl alcohol solution in the two containers 1 41 into the mixing section 53, and then discharge from the mixing section 53 into the container 3 61. The two pump bodies 2 52 can pump part of the catalytic solution in the container 2 42 into the throats 532 of the two mixing sections 53 (the principle of the mixing section 53 is derived from the Bernoulli principle. When the fluid passes through the throat 532, the cross-sectional area of ​​the pipeline gradually decreases and the flow rate increases. According to the Bernoulli equation, as the flow rate increases, , the pressure will decrease. Then, the fluid enters the diffuser 531, the cross-sectional area of ​​the pipeline increases, the flow rate slows down, and the pressure recovers), and mixes with the diester malonate solution and the p-nitrobenzyl alcohol solution in the two mixing sections 53 (the diester malonate solution or the p-nitrobenzyl alcohol solution reaches the throat 532 from the feed section 533, and the catalytic solution enters the throat 532. The spiral guide flange 534 in the throat 532 changes the flow direction of the fluid and guides the fluid to produce a vortex effect, thereby increasing the turbulence of the fluid and promoting the diester malonate solution to flow. liquid or a mixture of a p-nitrobenzyl alcohol solution and a catalytic solution), another pump body 2 52 directly pumps another part of the catalytic solution in the container 2 42 directly to the rotary joint 2 67. Based on the above scheme, part of the catalyst solution can be pumped into the mixing section 53 through the pump body 2 52 and efficiently contact and preliminarily react with the diester solution of malonic acid and the p-nitrobenzyl alcohol solution in a relatively short time, so that the catalyst can be fully dispersed at an early stage to avoid catalyst agglomeration or precipitation, and the contact area between the reactant and the catalyst can be enhanced. Since the catalyst and the reactant have been preliminarily mixed through the mixing section 53 before entering the container 3 61, the reactant has a better catalyst distribution when entering the container 3 61, which helps to accelerate the start of the reaction and shorten the mixing time. Compared with the traditional catalyst and reactant that start mixing in the agitator, this pre-mixing step can reduce the start time of the reaction and ensure faster entry into the reaction state. By adding the catalyst in two times (preliminary mixing with the reactant first and then adding the remaining part), more precise catalyst control can be achieved. The amount of catalyst introduced for the first time is relatively small, which can avoid premature overreaction of the catalyst or excessive local concentration, and control the initial rate of the reaction. The remaining catalyst can be evenly distributed in container three 61, ensuring that the catalyst concentration during the reaction is appropriate, and optimizing the continuity and yield of the reaction.

[0028] like Figure 1 and Figure 5As shown, the outer surface of one side of the shell 1 and the outer surface of one side of the side plate 2 are both connected with a lifting part 64, and the lifting part 64 includes two groups of fixed plates 641 respectively fixed on one side of the shell 1 and one side of the side plate 2, a motor 643 rotatably connected to a screw rod 642 and fixed to the outer surface of one side of the side plate 2 with one group of fixed plates 641, and a guide rod fixed to the other group of fixed plates 641, and the output shaft of the motor 643 passes through the fixed plate 641 and is connected to the screw rod 642, and movable grooves are opened inside the shell 1 and the side plate 2, and the two ends of the movable seat 65 extend outward through the movable grooves, and the extended end on one side of the movable seat 65 is screwed to the outside of the screw rod 642 and the extended end on the other side is movably sleeved on the outside of the guide rod.

[0029] By adopting the above technical solution, the motor 4 643 can drive the screw 642 to rotate, and the rotation of the screw 642 can drive the movable seat 65 to move up and down. The up and down movement of the movable seat 65 can drive the rod body 68, the shear plate 682 and the stator 3 69 to move up and down. The up and down movement of the shear plate 682 and the stator 3 69 can effectively promote the uniform distribution of the solvent and reactants in the reaction system. The up and down movement can effectively break the hierarchical structure of the solution, enhance the diffusion rate between the solute molecules and the solvent molecules, ensure that the reactants and the catalyst can contact quickly and evenly, and at the same time, it will continuously break the original flow field structure and promote the turbulent effect inside the fluid. This helps to mix materials more quickly and evenly, avoid liquid stratification or the formation of dead zones, improve the fluidity and uniformity of the entire reaction system, and can continuously disturb the fluid in the system to avoid the catalyst from aggregating in the low shear area, ensuring that the catalyst is continuously in an active reaction state.

[0030] like Fig. 9 As shown, a circulating defoaming unit 7 is also connected to the inside of the shell 1, and the circulating defoaming unit 7 includes two positioning plates 72 respectively fixed to the inner wall of the shell 1 and the inner wall of the side plate 2, a box body 71 located between the two positioning plates 72 and fixed to the two positioning plates 72 on both sides, a pump body four 74 and a pump body three 73 respectively fixed to the upper end and one side of the box body 71, a one-way exhaust valve 76 connected to the upper end of the box body 71, an ultrasonic generating part 75 fixed to the lower end of the box body 71, and the input end of the pump body three 73 is connected to the container three 61 and the output end is connected to the box body 71, and the input end of the pump body four 74 is connected to the box body 71 and the output end is connected to the container three 61.

[0031] By adopting the above technical solution, pump body three 73 can extract the solution at the bottom of container three 61 and pump it into box body 71, and pump body four 74 can pump the solution in box body 71 into the top of container three 61. By extracting the liquid at the bottom of container three 61 and re-discharging it into the top of container three 61, the liquid fluidity in the reaction chamber can be enhanced. After the bottom liquid is extracted and redirected to the top, it will naturally sink to the bottom of the reaction chamber through gravity and the driving action of the pump, forming a strong upward and downward circulation flow. This can accelerate the mixing of the components in the solution and improve the uniformity of the reaction. Since the solution in the container three 61 may generate bubbles when it is sheared and mixed at high speed, when the solution is pumped into the box body 71 by the pump body three 73, the ultrasonic generating part 75 at the bottom of the box body 71 (composed of structures such as an ultrasonic generator and an ultrasonic transducer, which are mature existing technologies and will not be described here) can promote the bubbles in the solution to aggregate into larger bubbles through ultrasonic oscillation, prompting the bubbles to be discharged from the solution and the gas to be discharged from the one-way exhaust valve 76, thereby avoiding the bubbles that may affect the uniformity of the reaction, and may cause temperature fluctuations or pressure changes, and even affect the separation and purification process. At the same time, the high-frequency vibration of the ultrasonic wave also helps to accelerate the dissolution of the reactants.

[0032] Method of use: Add malonic acid diester and p-nitrobenzyl alcohol into two containers 41 respectively, add catalyst into container 2 42, and then add solvent into two containers 41 and container 2 42. Motor 1 411 and motor 2 421 work to drive rotor 1 412 and rotor 2 422 to rotate respectively. Rotor 1 412 and rotor 2 422 rotate at high speed in coordination with stator 1 413 and stator 2 423 respectively, generating strong shear force, so that malonic acid diester and solvent, p-nitrobenzyl alcohol and solvent, catalyst and solvent are pre-mixed and dissolved to obtain malonic acid diester solution, p-nitrobenzyl alcohol solution, and catalyst solution respectively. Two pump bodies 51 can respectively pump the malonic acid diester solution and p-nitrobenzyl alcohol solution in the two containers 41 into two feeding parts 53. 3, the two pump bodies 2 52 can pump part of the catalytic solution in the container 2 42 into the throats 532 of the two mixing parts 53 and mix them with the diester solution of malonic acid and the p-nitrobenzyl alcohol solution in the two feeding parts 533, and then discharge them from the diffusion part 531 and enter the container 3 61 through the feeding port 2 63. The motor 5 661 drives the rod body 68 and the shearing piece 682 to rotate, and the shearing piece 682 rotates at a high speed with the stator 3 69 to generate a strong shearing force to mix the liquid in the container 3 61. The other pump body 2 52 directly pumps another part of the catalytic solution in the container 2 42 to the rotary joint 2 67. The catalyst solution fed into the rotary joint 2 67 is discharged from the discharge port 681 and quickly mixed and dissolved with the sheared solution in the container 3 61.

[0033] The above is only a preferred specific implementation of the present invention; however, the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical solution and its improved conception within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A thermal insulation preparation device for mono-p-nitrobenzyl malonate, comprising a housing (1), a side plate (2) fixed to one side of the housing (1), and three groups of feed ports (3) provided at the upper end of the housing (1), characterized in that: The shell (1) is internally connected with a pre-mixing unit (4) and a final mixing unit (6); the pre-mixing unit (4) comprises two raw material mixing components symmetrically connected to the shell (1) and a catalytic mixing component connected to the shell (1); the final mixing unit (6) is connected to the two raw material mixing components and the catalytic mixing component via a feeding portion (5); The raw material dissolving and mixing component comprises a container (41) fixedly connected to the inner wall of the shell (1), a stator (413) fixedly connected to the inner wall of the shell (1) and located inside the container (41), a motor (411) fixedly connected to the outer surface of the upper end of the shell (1), and a rotor (412) having one end fixedly connected to the output shaft of the motor (411) and the other end rotatably connected to the stator (413); The catalytic dissolving and mixing assembly comprises a second container (42) fixedly connected to the inner wall of the shell (1) and located between the two first containers (41), a second stator (423) fixedly connected to the inner wall of the shell (1) and located inside the second container (42), a second motor (421) fixedly connected to the outer surface of the upper end of the shell (1), and a second rotor (422) having one end fixedly connected to the output shaft of the second motor (421) and the other end rotatably connected to the second stator (423); The feeding section (5) comprises two mixing sections (53) symmetrically fixed to the upper end of the support plate (11), a pump body (51) fixed to the lower ends of the two containers (41) and connected to the output end of the container (41), three pump bodies (52) fixed to the lower ends of the container (42) and connected to the three output ends at the bottom of the container (42), two groups of support plates (54) fixed to the inner walls of the shell (1) and the side plate (2), and two rotary joints (58) fixed to the two groups of support plates (54), respectively. The mixing section (53) comprises a feeding section (533), a throat section (532) and a diffusion section (531), wherein the output ends of two pump bodies (52) are respectively connected to the two throat sections (532), the output ends of two pump bodies (51) are respectively connected to the input ends of two rotary joints (58), and the output end of another pump body (52) is connected to the input end of a rotary joint (67).

2. The thermal insulation preparation device of mono-p-nitrobenzyl malonate according to claim 1, characterized in that: The inner wall of the shell (1) is fixedly connected to a support plate (11), and two feed ports (63) connected to the feeding portion (5) are symmetrically provided in the support plate (11). The final dissolving and mixing unit (6) comprises a container (61) fixedly connected to the lower end of the support plate (11), a guide rod (611) fixedly connected to the inner bottom wall of the container (61), a rod body (68) movably sleeved on the outside of the guide rod (611), a movable seat (65) movably connected to the inside of the shell (1), and a rotary joint (67) fixedly connected to the upper end of the movable seat (65) and connected to the feeding portion (5). ), a hollow cavity formed inside the rod body (68) and a discharge port (681) formed on the outer surface of the rod body (68) and communicating with the hollow cavity, a stator three (69) fixedly connected to the lower end of the movable seat (65) and penetrating through the support plate (11) and extending into the interior of the container three (61), a shearing piece (682) fixedly connected to the outside of the rod body (68) and located inside the stator three (69), a driving part (66) connected to the inside of the movable seat (65) for driving the rod body (68) to rotate, and an inner tube of the rotary joint two (67) inserted into the hollow cavity and fixedly connected to the inner wall of the hollow cavity.

3. The thermal insulation preparation device of mono-p-nitrobenzyl malonate according to claim 2, characterized in that: The other end of the rod body (68) is rotatably connected to the inside of the movable seat (65), and the driving part (66) includes a motor five (661) fixedly connected to the upper end of the movable seat (65), a gear three (662) rotatably connected to the inside of the movable seat (65) and fixedly connected to the output shaft of the motor five (661), and a gear four (663) rotatably connected to the inside of the movable seat (65) and fixedly connected to the outer surface of the rod body (68), and the gear three (662) is meshed with the gear four (663).

4. The thermal insulation preparation device of mono-p-nitrobenzyl malonate according to claim 3, characterized in that: A heating jacket (62) is fixedly connected to the outer surface of the container three (61).

5. The thermal insulation preparation device of mono-p-nitrobenzyl malonate according to claim 4, characterized in that: A spiral guide flange (534) is integrally formed inside the throat portion (532); the upper ends of the two feeding portions (533) are rotatably connected to gear 2 (57); the upper ends of the two groups of support plates (54) are respectively fixedly connected to two motors 3 (55); and the lower ends of the two groups of support plates (54) are respectively rotatably connected to two gears 1 (56) meshing with gear 2 (57); the output shaft of motor 3 (55) passes through the support plate (54) and is connected to gear 1 (56); and gear 2 (57) is fixedly sleeved on the outside of the inner tube of rotary joint 1 (58).

6. The thermal insulation preparation device of mono-p-nitrobenzyl malonate according to claim 5, characterized in that: The outer surface of one side of the shell (1) and the outer surface of one side of the side plate (2) are both connected to a lifting part (64), and the lifting part (64) comprises two groups of fixed plates (641) respectively fixed to one side of the shell (1) and one side of the side plate (2), a motor four (643) fixed to the outer surface of one side of the side plate (2), and a guide rod fixed to the other group of fixed plates (641), and the output shaft of the motor four (643) passes through the fixed plate (641) and is connected to the screw rod (642), and the shell (1) and the side plate (2) are both provided with movable grooves, and the two ends of the movable seat (65) extend outward through the movable grooves, and the extension end of one side of the movable seat (65) is screwed to the outside of the screw rod (642) and the extension end of the other side is movably sleeved on the outside of the guide rod.

7. The thermal insulation preparation device of mono-p-nitrobenzyl malonate according to claim 6, characterized in that: A circulating defoaming unit (7) is also connected to the inside of the shell (1), and the circulating defoaming unit (7) comprises two positioning plates (72) respectively fixed to the inner wall of the shell (1) and the inner wall of the side plate (2), a box body (71) located between the two positioning plates (72) and respectively fixed to the two positioning plates (72) on both sides, a pump body four (74) and a pump body three (73) respectively fixed to the upper end and one side of the box body (71), a one-way exhaust valve (76) connected to the upper end of the box body (71), and an ultrasonic generating part (75) fixed to the lower end of the box body (71), wherein the input end of the pump body three (73) is connected to the container three (61) and the output end is connected to the box body (71), and the input end of the pump body four (74) is connected to the box body (71) and the output end is connected to the container three (61).

8. The thermal insulation preparation device of mono-p-nitrobenzyl malonate according to claim 7, characterized in that: A conical material discharge tray (415) is also fixedly connected to the interior of the container one (41), and a hollow groove is opened in the middle of the conical material discharge tray (415). The rotor one (412) is located in the hollow groove, and the gap between the inner wall of the hollow groove and the outside of the rotor one (412) is used for material discharge. A plurality of material discharge rods (416) are fixedly connected to the outside of the rotor one (412), and the lower ends of the material discharge rods (416) are in contact with the upper surface of the conical material discharge tray (415).

9. The thermal insulation preparation device of mono-p-nitrobenzyl malonate according to claim 8, characterized in that: A plurality of material distribution rods (414) are fixedly connected to the outside of the rotor 1 (412), and the plurality of material distribution rods (414) are located below the conical material discharge tray (415).

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