A neutralization distillation apparatus for N,N-diisopropylethylamine

Abstract

The utility model discloses a kind of N, N-diisopropyl ethylamine neutralization distillation device, it is related to neutralization distillation technical field, the N, N-diisopropyl ethylamine neutralization distillation device, including neutralization reaction kettle, stirring mechanism and lye distribution mechanism are equipped in neutralization reaction kettle, lye distribution mechanism is installed in the upper portion of neutralization reaction kettle, it is arranged horizontally annularly, the lower end of lye distribution mechanism is fixedly connected with the upper end of stirring mechanism, and lye distribution mechanism is rotated simultaneously when driving stirring mechanism rotation, it is even sprayed into reaction liquid phase area in circumferential direction multiple points to alkali liquor, the efficient dispersion and mixing of alkali liquor are realized.The utility model is rotated by the synergistic effect of multiple point injection lye distribution mechanism and micro rectifier structure, realize the spatial uniform distribution and rapid mixing of alkali liquor in reaction system, effectively avoid local over-alkali, improve the uniformity, stability and product yield of neutralization reaction.

Description

Technical Field

[0001] This utility model relates to the field of neutralization distillation technology, and in particular to an N,N-diisopropylethylamine neutralization distillation apparatus. Background Technology

[0002] In the synthesis of N,N-diisopropylethylamine, the amination reaction is often accompanied by the formation of acidic byproducts such as hydrobromic acid, which need to be neutralized to ensure the smooth progress of subsequent distillation and purification.

[0003] Traditional neutralization processes often involve adding alkali solution at a single point within the reactor, accompanied by mechanical stirring for mixing. However, concentrated injection of alkali solution can easily create localized high-pH areas, leading to localized over-alkaliness and causing hydrolysis, emulsification, or an increase in side reactions of the target product. Furthermore, since acid-base neutralization reactions are highly exothermic, uneven mixing can easily cause temperature fluctuations, further affecting reaction stability and reducing product yield and purity.

[0004] In addition, the existing equipment has fixed and uniform alkaline spray nozzles, and the stirring system and feeding system operate independently, making it difficult to achieve dynamic coordination between feeding and mixing, resulting in a long neutralization reaction cycle and poor uniformity. Utility Model Content

[0005] This invention provides an N,N-diisopropylethylamine neutralization distillation apparatus, including a neutralization reaction vessel. The neutralization reaction vessel is equipped with a stirring mechanism and an alkali distribution mechanism. The alkali distribution mechanism is installed on the upper part of the neutralization reaction vessel and arranged in a horizontal ring. The lower end of the alkali distribution mechanism is fixedly connected to the upper end of the stirring mechanism. When the alkali distribution mechanism rotates, it synchronously drives the stirring mechanism to rotate, so as to uniformly spray the alkali into the reaction liquid phase region at multiple points in the circumferential direction, thereby achieving efficient dispersion and mixing of the alkali.

[0006] Preferably, the liquid outlet pipe of the neutralization reactor is connected to the liquid inlet of the transfer pump via a pipeline, and the liquid outlet of the transfer pump is connected to the liquid inlet of the distillation column via a pipeline.

[0007] Preferably, the alkali distribution mechanism includes an inlet pipe, one end of which is rotatably connected to the top of the neutralization reactor and extends downward. An end cap is connected to the lower end of the inlet pipe, and a conical outlet pipe is provided at the lower end of the end cap. Several outlet holes are opened on the outer side of the outlet pipe for spraying the alkali solution out at multiple points.

[0008] Preferably, the upper end of the inlet pipe is rotatably connected to the lower end of the connecting pipe via a rotary joint, and the other end of the connecting pipe is connected to an automatic metering pump via a corrosion-resistant hose. The automatic metering pump is controlled by a pH feedback signal and continuously delivers alkaline solution to the inlet pipe.

[0009] Preferably, the outer wall of the inlet pipe is connected to an annular pipe, which is in communication with the inside of the inlet pipe. Multiple outlet pipes are evenly distributed along the circumference of the annular pipe to expand the distribution range of the alkali solution.

[0010] Preferably, the second outlet pipe includes an upper straight pipe section and a lower flared section. The straight pipe section is equipped with a micro rectifier core, which has a porous honeycomb structure and is used for preliminary rectification and flow equalization of the alkaline solution.

[0011] Preferably, the lower end of the first outlet pipe is provided with a flow guide shroud, which is inverted conical in shape and fixed to the outer periphery of the first outlet pipe to guide the alkaline solution to flow downward.

[0012] Preferably, a driven wheel is fixed to the outer wall of the liquid inlet pipe, and a driving wheel is rotatably installed on the top cover of the neutralization reactor. The driving wheel is driven by a drive motor and meshes with the driven wheel for transmission. Protective covers are provided on the outside of the driving wheel and the driven wheel to prevent foreign objects from entering.

[0013] Preferably, the stirring mechanism includes a stirring shaft fixedly connected to the lower end of the liquid outlet pipe, an inclined blade is provided at the upper end of the stirring shaft, and an anchor blade is provided at the lower end of the stirring shaft.

[0014] Preferably, a pH sensor is installed in the lower part of the side wall of the neutralization reactor, with its detection end extending below the liquid surface to avoid the stirring vortex zone and the alkali spray zone. It is used to monitor the pH value of the reaction system in real time and feed the signal back to the control system of the automatic metering pump to realize closed-loop regulation of the amount of alkali added.

[0015] This utility model provides an N,N-diisopropylethylamine neutralization distillation apparatus, which, compared with the prior art, offers the following advantages: 1. This utility model improves the uniformity of alkali distribution in the reaction system by setting a rotary annular alkali distribution mechanism combined with a multi-point spray and linkage stirring structure. After the alkali enters the annular distribution system through the inlet pipe, it is sprayed out synchronously in the circumferential direction through the outlet pipe and multiple sets of outlet holes on the annular pipe, realizing multi-point feeding in space. At the same time, the alkali distribution mechanism rotates under the drive of the driving wheel and the driven wheel, driving the jet flow to form a circumferential sweeping motion, avoiding the problem of excessively high local concentration caused by traditional single-point feeding. With the help of the inverted conical guide hood to guide the liquid flow direction, it prevents the alkali from accumulating on the liquid surface and ensures that it quickly cuts into the reaction liquid phase zone. It fundamentally solves the technical problems of local over-alkali, increased side reactions and product decomposition caused by uneven mixing during the neutralization process, and improves the reaction stability and product yield.

[0016] 2. This invention incorporates a porous honeycomb structured micro-rectifier core within the straight section of the outlet pipe to perform primary flow equalization and rectification of the sprayed alkali solution, eliminating velocity deviation and jet skew, and enhancing initial mixing efficiency. The rectifier core works synergistically with the rotating jet structure to form a fine and uniform micro-jet cluster before the alkali solution enters the main reaction zone, increasing the contact interface between the alkali solution and the hydrobromic acid-containing material, shortening the mixing time, and effectively ensuring the stable progress of the neutralization reaction. This provides a high-quality, low-impurity precursor solution for subsequent distillation and purification. Attached Figure Description

[0017] To more clearly illustrate the technical solutions of the embodiments of this utility model, the drawings used in the embodiments will be briefly introduced below. It should be understood that the following drawings only show some embodiments of this utility model and should not be regarded as a limitation of the scope. For those skilled in the art, other related drawings can be obtained from these drawings without creative effort.

[0018] Figure 1 This is a schematic diagram of the overall structure of an embodiment of the present utility model; Figure 2 This is a schematic diagram of the neutralization reactor structure according to an embodiment of the present invention; Figure 3 This is a top view of the neutralization reactor structure according to an embodiment of the present invention; Figure 4 The following is an embodiment of this utility model Figure 3 sectional view of the structure at point AA; Figure 5 This is a schematic diagram of the structure of the alkali distribution mechanism and other components according to an embodiment of the present invention; Figure 6 This is a schematic diagram showing the disassembled alkali distribution mechanism according to an embodiment of the present invention; Figure 7 This is a cross-sectional schematic diagram of the liquid outlet pipe according to an embodiment of the present utility model; Figure 8 This is a cross-sectional schematic diagram of the liquid outlet pipe of an embodiment of the present invention.

[0019] Figure label: 1. Neutralization reactor; 2. Transfer pump; 3. Distillation column; 4. pH sensor; 5. Inlet pipe; 6. End cap; 7. Outlet pipe one; 8. Flow guide; 9. Connecting pipe; 10. Drive wheel; 11. Driven wheel; 12. Annular pipe; 13. Outlet pipe two; 14. Rectifier core; 15. Stirring shaft; 16. Inclined blade impeller; 17. Anchor impeller; 18. Drive motor; 19. Protective cover. Detailed Implementation

[0020] The following detailed description, in conjunction with the accompanying drawings, outlines some embodiments of the present invention. Unless otherwise specified, the following embodiments and features can be combined with each other.

[0021] Please refer to Figures 1-8 This utility model provides an N,N-diisopropylethylamine neutralization distillation apparatus, including a neutralization reactor 1 and an independently set distillation column 3. The neutralization reactor 1 is used to complete the neutralization reaction of the hydrobromic acid-containing reaction solution. It is provided with a liquid outlet pipe at the bottom, which is connected to the liquid inlet of a transfer pump 2 through a pipeline. The liquid outlet of the transfer pump 2 is connected to the feed inlet of the distillation column 3 through a pipeline, which is used to transport the neutralized material to the distillation column 3 for separation and purification.

[0022] refer to Figure 3 The neutralization reactor 1 is equipped with a stirring mechanism and an alkali distribution mechanism. The alkali distribution mechanism is installed on the upper part of the neutralization reactor 1 and is arranged in a horizontal ring. The alkali distribution mechanism includes a vertically arranged inlet pipe 5. The upper end of the inlet pipe 5 passes through the top cover of the neutralization reactor 1 and is rotatably connected to the lower end of the external connecting pipe 9 through a rotary joint. The other end of the connecting pipe 9 is connected to an automatic metering pump through a corrosion-resistant fluoroplastic hose. The automatic metering pump is controlled by a pH feedback signal and can accurately adjust the delivery flow rate of alkali solution such as NaOH solution.

[0023] The inlet pipe 5 extends downward into the interior of the neutralization reactor 1, and its lower end is sealed with an end cap 6. The lower part of the end cap 6 is provided with a downward-extending conical outlet pipe 7. Multiple outlet holes are evenly opened on the outer wall of the outlet pipe 7 along the circumferential direction to spray the alkaline solution out simultaneously at multiple points in the circumferential direction.

[0024] like Figure 8 As shown, an annular pipe 12 is also fixedly connected to the outer wall of the inlet pipe 5. The annular pipe 12 is connected to the inside of the inlet pipe 5. Multiple outlet pipes 13 are evenly distributed along the circumferential direction on it. Each outlet pipe 13 includes an upper straight pipe section and a lower flared section. A micro rectifier core 14 is embedded in the straight pipe section. The rectifier core 14 is made of polytetrafluoroethylene material and has a porous honeycomb structure. It is used for primary rectification and flow equalization of the alkaline solution, preventing jet deflection and improving the initial mixing efficiency.

[0025] A flow guide shroud 8 is fixed at the lower end of the outlet pipe 7. The flow guide shroud 8 is in the shape of an inverted cone and is placed around the outlet area to guide the alkaline solution to flow downward, prevent it from accumulating or splashing on the liquid surface, and ensure that the alkaline solution quickly enters the reaction liquid phase zone.

[0026] A driven wheel 11 is fixed to the outer wall of the liquid inlet pipe 5. A driving wheel 10 is rotatably installed on the top cover of the neutralization reactor 1. The driving wheel 10 is driven by the drive motor 18 and meshes with the driven wheel 11 to drive the alkali distribution mechanism and the stirring mechanism fixedly connected to it to rotate as a whole. Stainless steel protective covers 19 are provided on the outside of the driving wheel 10 and the driven wheel 11 to prevent foreign objects from falling into the meshing area and to ensure transmission safety.

[0027] refer to Figure 5 The stirring mechanism includes a stirring shaft 15 fixedly connected to the lower end of the outlet pipe 7. The upper part of the stirring shaft 15 is provided with an inclined blade 16 and the lower part is provided with an anchor blade 17. The inclined blade 16 is used to generate axial flow and promote vertical circulation. The anchor blade 17 rotates close to the reactor wall to prevent the alkaline solution from short-circuiting along the wall and enhance the mixing effect in the near-wall area.

[0028] A pH sensor 4 is installed on the lower part of the side wall of the neutralization reactor 1. Its detection end extends 250mm below the liquid surface, avoiding the stirring vortex zone and the alkali spray zone. It is used to monitor the pH value of the reaction system in real time. The signal of the pH sensor 4 is connected to the PLC control system to form a closed-loop regulation with the automatic metering pump. When the pH is lower than the set value, alkali addition is started and stopped after the target value is reached, so as to achieve precise control of the amount of alkali added.

[0029] In summary, after the hydrobromic acid-containing reaction solution is added to the neutralization reactor 1, the drive motor 18 starts, driving the drive wheel 10 to rotate. Through gear transmission, the driven wheel 11 and the inlet pipe 5 rotate as a whole. According to the feedback signal from the pH sensor 4, the automatic metering pump continuously delivers the alkaline solution to the inlet pipe 5 through the hose, connecting pipe 9, and rotary joint. The alkaline solution is sprayed out at multiple points in the circumferential direction through the first outlet pipe 7 and the second outlet pipe 13 on the annular pipe 12. With the help of the rectifier core 14 and the guide shroud 8, it achieves uniform distribution. At the same time, the stirring mechanism rotates synchronously to enhance mixing. After neutralization, the material is sent to the distillation tower 3 by the conveying pump 2 for separation and purification.

[0030] The above are merely preferred embodiments of this utility model and are not intended to limit the scope of this utility model. Various modifications and variations can be made to this utility model by those skilled in the art. Any modifications, equivalent substitutions, or improvements made within the spirit and principles of this utility model should be included within the protection scope of this utility model.

Claims

1. An N,N-diisopropylethylamine neutralization distillation apparatus, characterized in that: The system includes a neutralization reactor (1), which is equipped with a stirring mechanism and an alkali distribution mechanism. The alkali distribution mechanism is installed on the upper part of the neutralization reactor (1) and arranged in a horizontal ring. The lower end of the alkali distribution mechanism is fixedly connected to the upper end of the stirring mechanism. When the alkali distribution mechanism rotates, it synchronously drives the stirring mechanism to rotate, so that the alkali is evenly sprayed into the reaction liquid phase area at multiple points in the circumferential direction, thereby achieving efficient dispersion and mixing of the alkali.

2. The N,N-diisopropylethylamine neutralization distillation apparatus according to claim 1, characterized in that: The liquid outlet pipe of the neutralization reactor (1) is connected to the liquid inlet of the transfer pump (2) through a pipeline, and the liquid outlet of the transfer pump (2) is connected to the liquid inlet of the distillation tower (3) through a pipeline.

3. The N,N-diisopropylethylamine neutralization distillation apparatus according to claim 1, characterized in that: The alkali distribution mechanism includes an inlet pipe (5), one end of which is rotatably connected to the top of the neutralization reactor (1) and extends downward. The lower end of the inlet pipe (5) is connected to an end cap (6), and the lower end of the end cap (6) is provided with a conical outlet pipe (7). Several outlet holes are opened on the outside of the outlet pipe (7) for spraying the alkali solution out at multiple points.

4. The N,N-diisopropylethylamine neutralization distillation apparatus according to claim 3, characterized in that: The upper end of the inlet pipe (5) is rotatably connected to the lower end of the connecting pipe (9) through a rotary joint. The other end of the connecting pipe (9) is connected to the automatic metering pump through a corrosion-resistant hose. The automatic metering pump is controlled by the pH feedback signal and continuously delivers the alkaline solution to the inlet pipe (5).

5. The N,N-diisopropylethylamine neutralization distillation apparatus according to claim 4, characterized in that: The outer wall of the inlet pipe (5) is connected to an annular pipe (12), which is connected to the inside of the inlet pipe (5). Multiple outlet pipes (13) are evenly distributed along the circumference of the annular pipe (12) to expand the distribution range of the alkali solution.

6. The N,N-diisopropylethylamine neutralization distillation apparatus according to claim 5, characterized in that: The second outlet pipe (13) includes an upper straight pipe section and a lower flared section. The straight pipe section is equipped with a micro rectifier core (14), which has a porous honeycomb structure and is used for preliminary rectification and equalization of the alkaline solution.

7. The N,N-diisopropylethylamine neutralization distillation apparatus according to claim 6, characterized in that: The lower end of the outlet pipe (7) is provided with a flow guide (8), which is inverted cone-shaped and fixed to the outer periphery of the outlet pipe (7) to guide the alkaline solution to flow downward.

8. The N,N-diisopropylethylamine neutralization distillation apparatus according to claim 7, characterized in that: The outer wall of the liquid inlet pipe (5) is fixed with a driven wheel (11), and the top cover of the neutralization reactor (1) is rotatably mounted with a driving wheel (10). The driving wheel (10) is driven by a drive motor (18) and meshes with the driven wheel (11). The outer sides of the driving wheel (10) and the driven wheel (11) are provided with protective covers (19) to prevent foreign objects from entering.

9. The N,N-diisopropylethylamine neutralization distillation apparatus according to claim 3, characterized in that: The stirring mechanism includes a stirring shaft (15) fixedly connected to the lower end of the liquid outlet pipe (7), with an inclined blade (16) at the upper end of the stirring shaft (15) and an anchor blade (17) at the lower end of the stirring shaft (15).

10. The N,N-diisopropylethylamine neutralization distillation apparatus according to claim 1, characterized in that: A pH sensor (4) is installed in the lower part of the side wall of the neutralization reactor (1). Its detection end extends into the liquid surface to avoid the stirring vortex zone and the alkali spray zone. It is used to monitor the pH value of the reaction system in real time and feed the signal back to the control system of the automatic metering pump to realize the closed-loop regulation of the amount of alkali added.

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