A neutralization separation column for synthesizing trioctyl phosphate

Abstract

The utility model provides a kind of neutralization separating tower for synthesizing trioctyl phosphate, including tower body, the inner upper portion of the tower body is provided with lye distribution assembly, the inner lower portion of the tower body is provided with static stratification space, the static stratification space of the tower body is fixedly provided with floating type supernatant separating assembly, to solve the problem that ordinary separating tower in prior art cannot maintain stable oil-water interface when trioctyl phosphate synthesis neutralization is carried out due to large lye consumption when feed flow or composition fluctuates, leading to unstable separation operation, the tower body with floating type supernatant separating assembly is designed, by the setting of floating type supernatant separating assembly, the height position of suction head can be automatically adjusted, so that it always floats at the interface of upper liquid, to adapt to liquid level change in real time, maintain stable separation operation, solve the problem of separation efficiency decline or mixing caused by liquid level fluctuation.

Description

Technical Field

[0001] This application relates to the technical field of trioctyl phosphate synthesis and separation equipment, and in particular to a neutralization separation tower for the synthesis of trioctyl phosphate. Background Technology

[0002] Trioctyl phosphate, as an important chemical product, is widely used in plasticizers, extractants and flame retardants. Its synthesis process usually involves esterification reaction. The acidic crude product produced after the reaction needs to be neutralized with alkaline solution to remove residual acidic catalyst and reaction by-products. The neutralized mixture is an oil-water two-phase system, mainly consisting of the upper trioctyl phosphate organic phase and the lower salt water phase.

[0003] In existing technologies, the commonly used neutralization separation towers are usually packed towers or plate towers. The alkaline solution is sprayed from the top through a distributor and undergoes mass transfer and reaction with the organic phase material entering from the middle or top of the tower in the packing layer or on the tower plate. The mixed liquid after the reaction is allowed to stand and separate into layers at the bottom of the tower, and the upper organic phase is collected through an outlet pipeline set at a fixed height.

[0004] However, in actual industrial operation, this separation method inevitably encounters fluctuations in feed flow rate, temperature, or material composition during production, causing changes in the liquid level inside the reboiler. The fixed outlet cannot adapt to these dynamically changing liquid levels. When the liquid level is too low, the outlet may be exposed to the gas phase, leading to pump cavitation or gas intrusion, disrupting operational continuity. When the liquid level is too high, the outlet may be submerged in the lower aqueous phase, causing the aqueous phase to mix with the organic phase product, resulting in product contamination, quality degradation, and increased subsequent refining load.

[0005] In other words, existing technologies suffer from the following technical problems: in the synthesis of trioctyl phosphate, conventional separation towers cannot adaptively adjust the extraction height, making it difficult to maintain a stable oil-water interface during feed fluctuations, resulting in unstable separation operations and decreased product purity. Therefore, a neutralization separation tower for the synthesis of trioctyl phosphate is proposed to address these issues. Utility Model Content

[0006] This embodiment provides a neutralization separation tower for the synthesis of trioctyl phosphate to solve the problem that ordinary separation towers in the prior art have difficulty maintaining a stable oil-water interface when the feed fluctuates.

[0007] A neutralization separation tower for synthesizing trioctyl phosphate includes a tower body, an alkali distribution component is provided in the upper part of the tower body, the alkali distribution component is used to distribute and spray the alkali solution, and a packing layer is fixed in the middle of the inner cavity of the tower body. The feature is that: a static layering space is provided in the lower part of the tower body, and a floating upper liquid separation component is fixedly installed in the static layering space of the tower body. The floating upper liquid separation component consists of a movable guide sleeve and a suction head fixed to the guide sleeve. A floating cylinder is also provided on the guide sleeve. When the liquid level at the bottom of the tower body is changing, the floating cylinder adaptively moves to adjust the height of the suction head.

[0008] The neutralization and separation tower for synthesizing trioctyl phosphate is characterized in that: a fixed base is fixedly connected to the bottom of the tower body, and an organic material inlet is fixedly connected to the upper end of the inner cavity of the tower body.

[0009] The neutralization and separation tower for synthesizing trioctyl phosphate is characterized in that: the alkali distribution assembly includes an input pipe, a circular shell, and a dispersion pipe. The circular shell is located at the center of the upper part of the tower body. Multiple dispersion pipes are arranged around the side wall of the circular shell. Multiple spray heads are provided at the bottom of each dispersion pipe. One end of the input pipe is connected to the circular shell, and the other end of the input pipe extends out of the tower body along the side wall.

[0010] The neutralization and separation tower for synthesizing trioctyl phosphate is characterized in that: a flow guiding structure is provided between the packing layer and the static stratification space, the flow guiding structure includes a flow guiding inclined plate and a flow guiding pipe, the flow guiding inclined plate is fixed to the inner wall of the tower body, the flow guiding inclined plate is inclined, and the lower end of the lowest point of the flow guiding inclined plate is fixedly connected to a flow guiding pipe that penetrates the top surface of the flow guiding inclined plate, and the bottom end of the flow guiding pipe extends into the bottom static stratification space of the tower body.

[0011] The neutralization and separation tower for synthesizing trioctyl phosphate is characterized in that: a plurality of baffles extending from opposite sides of the inner cavity of the guide tube are fixedly and alternately arranged in the inner cavity of the guide tube.

[0012] The neutralization separation tower for synthesizing trioctyl phosphate is characterized in that: the guide sleeve is fitted on the outer wall of the fixed guide rod and slides between the guide sleeve and the fixed guide rod; the bottom end of the fixed guide rod is fixedly connected to the inner bottom of the tower body; the top end of the fixed guide rod is fixedly connected to a fixed bracket A; the fixed bracket A is fixedly connected to the side wall of the tower body; and a floating cylinder is fixedly connected to the side wall of the guide sleeve.

[0013] The neutralization separation tower for synthesizing trioctyl phosphate is characterized in that: one end of a fixed support B is fixedly connected to the side wall of the guide sleeve, the other end of the fixed support B is fixedly connected to a longitudinally arranged suction pipe, the bottom end of the suction pipe is fixedly connected to a suction head, the top end of the suction pipe is fixedly connected to one end of a connecting hose, the other end of the connecting hose is fixedly connected to one end of an output pipe, and the other end of the output pipe penetrates the side wall of the tower body and extends to the outside of the wall.

[0014] The neutralization separation tower for synthesizing trioctyl phosphate is characterized in that: a sleeve is fitted around the outside of the connecting hose, the outer wall of the sleeve is fixedly connected to the output pipe, and a sliding plate is fixedly fitted around the top of the suction pipe, the sliding plate being slidably fitted inside the sleeve.

[0015] The neutralization separation tower for synthesizing trioctyl phosphate is characterized in that: a leakage hole is provided on the sliding plate.

[0016] The neutralization and separation tower for synthesizing trioctyl phosphate is characterized in that a wastewater outlet is provided at the lower end of the side wall of the tower body.

[0017] In order to solve the problem in the prior art that ordinary separation towers may not be able to maintain a stable oil-water interface when the feed flow rate or composition fluctuates during the neutralization of trioctyl phosphate synthesis due to the large consumption of alkali, thus leading to unstable separation operation, this application designs a tower with a floating upper liquid separation component. By setting the floating upper liquid separation component, the height of the suction head can be automatically adjusted so that it always floats at the interface of the upper liquid, thereby adapting to changes in the liquid level in real time and maintaining a stable separation operation, solving the problem of decreased separation efficiency or mixing caused by liquid level fluctuations. Attached Figure Description

[0018] To more clearly illustrate the technical solutions in the embodiments of this application or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0019] Figure 1 This is a schematic diagram of the overall structure of this utility model; Figure 2 This is a front view structural diagram of the present utility model; Figure 3 This is a schematic diagram of the internal structure of the present invention; Figure 4 This is a schematic diagram of the internal planar structure of the present invention; Figure 5 This is a schematic diagram of the internal structure of the floating upper liquid separation component of this utility model; Figure 6 This is a schematic diagram of the internal structure of the flow guiding structure of this utility model.

[0020] In the diagram: 1. Tower body; 101. Organic material inlet; 2. Alkali distribution assembly; 201. Input pipe; 202. Circular shell; 203. Dispersion pipe; 204. Spray head; 3. Packing layer; 4. Flow guiding structure; 401. Flow guiding inclined plate; 402. Flow guiding pipe; 403. Baffle plate; 5. Floating upper liquid separation assembly; 501. Fixed support A; 502. Fixed guide rod; 503. Guide sleeve; 504. Floating cylinder; 505. Fixed support B; 506. Suction pipe; 507. Suction head; 508. Sleeve; 509. Sliding plate; 5091. Leakage hole; 510. Output pipe; 511. Connecting hose; 6. Wastewater outlet; 7. Fixed base. Detailed Implementation

[0021] To enable those skilled in the art to better understand the present application, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present application, and not all embodiments. Based on the embodiments in the present application, all other embodiments obtained by those of ordinary skill in the art without creative effort should fall within the scope of protection of the present application.

[0022] Please see Figure 1 and Figure 2 As shown, a neutralization separation tower for synthesizing trioctyl phosphate includes a tower body 1, an alkaline solution distribution component 2 is provided in the upper part of the tower body 1, the alkaline solution distribution component 2 is used to distribute and spray the alkaline solution, and a packing layer 3 is fixed in the middle of the inner cavity of the tower body 1. The feature is that: a static layering space is provided in the lower part of the tower body 1, and a floating upper liquid separation component 5 is fixedly installed in the static layering space of the tower body 1. The floating upper liquid separation component 5 consists of a movable guide sleeve 503 and a suction head 507 fixed to the guide sleeve 503. A floating cylinder 504 is also provided on the guide sleeve 503. When the liquid level at the bottom of the tower body 1 is changing, the floating cylinder 504 adaptively moves to adjust the height of the suction head 507.

[0023] To address the problem in existing technologies where conventional separation towers, during the neutralization of trioctyl phosphate synthesis, suffer from high alkali consumption and may fail to maintain a stable oil-water interface when feed flow or composition fluctuates, leading to unstable separation operations, this application designs a tower body 1 with a floating upper liquid separation component 5. By setting up the floating upper liquid separation component 5, the height of the suction head 507 can be automatically adjusted to ensure it always floats at the interface of the upper liquid, thereby adapting to changes in the liquid level in real time and maintaining stable separation operations. This solves the problem of decreased separation efficiency or mixing caused by liquid level fluctuations.

[0024] As a further technical solution, see [link / reference] Figure 1 As shown, a fixed base 7 is fixedly connected to the bottom of the tower body 1, and an organic material inlet 101 is fixedly connected to the upper end of the inner cavity of the tower body 1. Through this technical solution, the fixed base 7 provides a stable support for the tower body 1, ensuring the structural stability and safety of the equipment during operation and preventing the separation effect from being affected by vibration or tilting. The organic material inlet 101 is used to introduce organic phase materials so that they can fully contact the alkaline solution in the tower.

[0025] As a preferred technical solution, please refer to Figure 2 and Figure 3 As shown, the alkali distribution assembly 2 includes an input pipe 201, a circular shell 202, and dispersion pipes 203. The circular shell 202 is located at the center of the upper part of the tower body 1. Multiple dispersion pipes 203 are arranged around the side wall of the circular shell 202. Multiple spray heads 204 are provided at the bottom of each dispersion pipe 203. One end of the input pipe 201 is connected to the circular shell 202, and the other end of the input pipe 201 extends out of the tower body 1 along the side wall. Through this technical solution, the alkali enters the circular shell 202 through the input pipe 201 and is evenly distributed to each dispersion pipe 203. Finally, it is sprayed out by the spray heads 204 in the form of atomization or dripping, so that the alkali is evenly distributed on the packing layer 3, increasing the contact area with the organic material and improving the efficiency and thoroughness of the neutralization reaction.

[0026] Specifically, to address the issue of uneven alkali distribution potentially leading to incomplete local reactions, the circular shell 202 and several radially distributed dispersion pipes 203 together form a ring-shaped distribution network structure. Spray heads 204 are evenly arranged on the dispersion pipes 203, with their spray angle covering the entire cross-section of the tower body 1. This arrangement ensures that the alkali solution can evenly cover the packing layer 3 below, thereby increasing the contact area between the gas and liquid phases and improving the efficiency and uniformity of the neutralization reaction.

[0027] For specific technical solutions, please refer to Figure 3 As shown, a flow guiding structure 4 is provided between the packing layer 3 and the static stratification space. The flow guiding structure 4 includes a flow guiding inclined plate 401 and a flow guiding pipe 402. The flow guiding inclined plate 401 is fixed to the inner wall of the tower body 1 and is inclined. The lower end of the lowest point of the flow guiding inclined plate 401 is fixedly connected to the flow guiding pipe 402, which penetrates the top surface of the flow guiding inclined plate 401. The bottom end of the flow guiding pipe 402 extends into the static stratification space at the bottom of the tower body 1. Through this technical solution, the flow guiding inclined plate 401 collects the liquid flowing down from the packing layer 3 and guides it smoothly into the flow guiding pipe 402. The flow guiding pipe 402 transports the liquid to the static stratification space at the bottom of the tower, avoiding direct liquid fall and causing turbulence, which is conducive to the stable stratification of the oil and water phases.

[0028] As a preferred technical solution, please refer to Figure 6As shown, several baffles 403 extending from opposite sides of the inner cavity of the guide tube 402 are also fixedly and alternately arranged in the inner cavity of the guide tube 402. Through this technical solution, the baffles 403 cause the liquid to undergo multiple deflections in the guide tube 402, reducing the liquid flow rate and kinetic energy, thereby reducing the impact on the liquid surface at the bottom of the tower, further promoting static stratification, and preventing the already stratified liquids from remixing.

[0029] As a further technical solution, see [link / reference] Figure 3 and Figure 4 As shown, the guide sleeve 503 is fitted onto the outer wall of the fixed guide rod 502 and slides with it. The bottom end of the fixed guide rod 502 is fixedly connected to the inner bottom of the tower body 1. The top end of the fixed guide rod 502 is fixedly connected to a fixed bracket A501, which is fixedly connected to the side wall of the tower body 1. A float cylinder 504 is fixedly connected to the side wall of the guide sleeve 503. Through this technical solution, the fixed guide rod 502 and the fixed bracket A501 provide a stable guiding structure. The guide sleeve 503 can slide up and down along the fixed guide rod 502, and the float cylinder 504 floats with the change of liquid level, thereby driving the entire separation assembly to adaptively adjust its height and ensure that the suction head 507 is always located at the upper liquid interface.

[0030] Specifically, to address the need for precise control of the immersion depth of the suction head 507 due to the density difference between the upper organic phase and the lower aqueous phase, the floating cylinder 504 can be made with a hollow, sealed structure or filled with low-density foam material. In practical implementation, its buoyancy is calculated and adjusted to ensure that the average density of the entire floating upper liquid separation assembly 5 is between that of the upper organic phase and the lower aqueous phase. This allows the suction head 507 to remain precisely suspended at the interface between the two liquid layers, ensuring its inlet is completely immersed in the upper organic phase for suction, while preventing the intake of the lower aqueous phase, thus achieving precise separation.

[0031] For specific technical solutions, please refer to Figure 3 and Figure 4 As shown, the side wall of the guide sleeve 503 is also fixedly connected to one end of the fixed bracket B505. The other end of the fixed bracket B505 is fixedly connected to a longitudinally arranged suction pipe 506. The bottom end of the suction pipe 506 is fixedly connected to a suction head 507. The top end of the suction pipe 506 is fixedly connected to one end of a connecting hose 511. The other end of the connecting hose 511 is fixedly connected to one end of an output pipe 510. The other end of the output pipe 510 penetrates the side wall of the tower body 1 and extends to the outside of the wall.

[0032] In practical use, one end of the output pipe 510 is connected to a suction device. The negative pressure generated by the suction device draws the upper liquid—specifically, the oily liquid with trioctyl phosphate as its main component—through the suction head 507. The liquid is then discharged from the tower sequentially through the suction pipe 506, the connecting hose 511, and the output pipe 510, achieving continuous separation. The connecting hose 511 has a certain degree of flexibility, allowing the suction head 507 to move with the float 504 without affecting the pipe connection.

[0033] As a preferred technical solution, a sleeve 508 is fitted onto the outside of the connecting hose 511. The outer wall of the sleeve 508 is fixedly connected to the output pipe 510. A sliding plate 509 is fixedly fitted onto the top of the suction pipe 506. The sliding plate 509 is slidably fitted inside the sleeve 508. A leakage hole 5091 is provided on the sliding plate 509. Through this technical solution, the sleeve 508 and the sliding plate 509 form a protective structure to prevent materials or impurities in the tower from directly impacting or entangled in the connecting hose 511. The leakage hole 5091 allows gas and liquid to pass through, reducing the resistance when the sliding plate 509 moves, while avoiding the hose from being deformed by pressure, ensuring a stable and reliable suction process.

[0034] Furthermore, to address the potential damage to the connecting hose 511 caused by long-term exposure to chemical environments due to friction with internal tower components, contact with chemicals, or liquid impact, the sleeve 508 forms a robust protective channel. The sliding plate 509 moves synchronously with the suction pipe 506, and its outer edge slides against the inner wall of the sleeve 508, creating a dynamic seal. The leakage hole 5091 on the sliding plate 509 balances the air pressure in the upper and lower parts of the sleeve 508, prevents the formation of air cushions or vacuum damping, and allows a small amount of liquid to pass through for lubrication and flushing. However, it effectively blocks most impurities and liquid flow from directly impacting the connecting hose 511, thereby extending the service life of the hose and improving the reliability of the system.

[0035] Preferably, to address the issue of efficient mass transfer and rapid separation between the organic phase and the alkali solution within the tower, the tower body 1 is configured from top to bottom as an alkali solution distribution zone, a packing reaction zone, a flow guiding zone, and a static separation zone. The organic phase material enters the upper part of the tower body 1 through the organic material inlet 101, while the alkali solution is sprayed downwards through the alkali solution distribution component 2. Both phases fully contact and neutralize on the surface of the packing layer 3. The resulting mixture is then smoothly guided into the static stratification space at the bottom of the tower via the flow guiding structure 4. Oil-water separation is achieved using density differences. The upper organic phase is continuously collected by the floating upper liquid separation component 5, while the lower aqueous phase is periodically discharged through the wastewater outlet 6 at the bottom of the tower. This structural layout enables continuous and highly efficient neutralization and separation.

[0036] The above are merely preferred embodiments of this application and are not intended to limit this application. Various modifications and variations can be made to this application by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of this application should be included within the protection scope of this application.

Claims

1. A neutralization separation tower for synthesizing trioctyl phosphate, comprising a tower body (1), wherein an alkali distribution component (2) is provided in the upper part of the tower body (1), the alkali distribution component (2) is used to distribute and spray the alkali solution, and a packing layer (3) is fixed in the middle of the inner cavity of the tower body (1). Its features are: The lower part of the tower body (1) is provided with a static layering space. A floating upper liquid separation component (5) is fixedly installed in the static layering space of the tower body (1). The floating upper liquid separation component (5) consists of a movable guide sleeve (503) and a suction head (507) fixed to the guide sleeve (503). A floating cylinder (504) is also provided on the guide sleeve (503). When the liquid level at the bottom of the tower body (1) is changing, the floating cylinder (504) adaptively moves to adjust the height of the suction head (507). The alkali distribution assembly (2) includes an input pipe (201), a circular shell (202), and a dispersion pipe (203). The circular shell (202) is located at the center of the upper part of the tower body (1). Multiple dispersion pipes (203) are arranged around the side wall of the circular shell (202). Multiple spray heads (204) are provided at the bottom of each dispersion pipe (203). One end of the input pipe (201) is connected to the circular shell (202), and the other end of the input pipe (201) extends along the side wall of the tower body (1) to the outside of the tower body (1). A flow guiding structure (4) is provided between the packing layer (3) and the static layered space. The flow guiding structure (4) includes a flow guiding inclined plate (401) and a flow guiding pipe (402). The flow guiding inclined plate (401) is fixed to the inner wall of the tower body (1). The flow guiding inclined plate (401) is inclined. The lower end of the lowest point of the flow guiding inclined plate (401) is fixedly connected to a flow guiding pipe (402) that penetrates the top surface of the flow guiding inclined plate (401). The bottom end of the flow guiding pipe (402) extends to the bottom static layered space of the tower body (1).

2. The neutralization separation tower for synthesizing trioctyl phosphate according to claim 1, characterized in that: The bottom of the tower body (1) is fixedly connected to a fixed base (7), and the upper end of the inner cavity of the tower body (1) is fixedly connected to an organic material inlet (101).

3. The neutralization separation tower for synthesizing trioctyl phosphate according to claim 1, characterized in that: The inner cavity of the guide tube (402) is also fixedly and alternately provided with a number of baffles (403) extending from opposite sides of the inner cavity of the guide tube (402) to the opposite side.

4. The neutralization separation tower for synthesizing trioctyl phosphate according to claim 1, characterized in that: The guide sleeve (503) is sleeved on the outer wall of the fixed guide rod (502) and slides between the fixed guide rod (502). The bottom end of the fixed guide rod (502) is fixedly connected to the inner bottom of the tower body (1). The top end of the fixed guide rod (502) is fixedly connected to a fixed bracket A (501). The fixed bracket A (501) is fixedly connected to the side wall of the tower body (1). The side wall of the guide sleeve (503) is fixedly connected to a floating cylinder (504).

5. The neutralization separation tower for synthesizing trioctyl phosphate according to claim 4, characterized in that: The side wall of the guide sleeve (503) is also fixedly connected to one end of the fixed bracket B (505). The other end of the fixed bracket B (505) is fixedly connected to a longitudinally arranged suction pipe (506). The bottom end of the suction pipe (506) is fixedly connected to a suction head (507). The top end of the suction pipe (506) is fixedly connected to one end of a connecting hose (511). The other end of the connecting hose (511) is fixedly connected to one end of an output pipe (510). The other end of the output pipe (510) penetrates the side wall of the tower body (1) and extends to the outside of the wall.

6. The neutralization separation tower for synthesizing trioctyl phosphate according to claim 5, characterized in that: The connecting hose (511) is fitted with a sleeve (508), the outer wall of the sleeve (508) is fixedly connected to the output pipe (510), and the top of the suction pipe (506) is fixedly fitted with a sliding plate (509), which is slidably fitted inside the sleeve (508).

7. The neutralization separation tower for synthesizing trioctyl phosphate according to claim 6, characterized in that: The sliding plate (509) is provided with a leakage hole (5091).

8. The neutralization separation tower for synthesizing trioctyl phosphate according to claim 1, characterized in that: Wastewater outlet (6) is provided at the lower end of the side wall of the tower body (1).

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