Water phase separation device for triethylamine

Abstract

The utility model relates to the technical field of triethylamine water removal, and discloses a triethylamine water phase separation device which comprises a tank body, a stirring part arranged in the tank body, and an oil phase discharge pipe, a water phase discharge pipe and a blow-off pipe which are arranged at the bottom of the tank body, the upper end of the oil phase discharging pipe and the upper end of the water phase discharging pipe both extend into the tank body, the upper end of the oil phase discharging pipe is higher than the upper end of the water phase discharging pipe, the upper end of the water phase discharging pipe is higher than the upper end of a prime number discharging pipe, and the oil phase discharging pipe, the water phase discharging pipe and the discharging pipe are all provided with opening and closing valves. According to the invention, a water phase and an oil phase can be separately discharged conveniently.

Description

Technical Field

[0001] This application relates to the technical field of triethylamine dehydration, and in particular to a triethylamine water phase separation device. Background Technology

[0002] Triethylamine is an important chemical raw material, widely used as a catalyst and acid-binding agent in the preparation of pesticides and pharmaceutical intermediates such as glyphosate, ethyl difluoroacetate, and 5-nonylsalicylaldehyde, generating triethylamine salt as a byproduct. Due to its high price and toxicity, triethylamine must be recovered from the byproduct triethylamine salt and reused in the main process.

[0003] The industrial triethylamine recovery process mainly consists of four steps:

[0004] 1. Neutralize the wastewater containing triethylamine salts with an alkaline solution of approximately 40% concentration;

[0005] 2. Distill the above wastewater to recover triethylamine. At this time, the triethylamine has a high water content.

[0006] 3. Dry the above-mentioned aqueous triethylamine in a phase separation tank with solid sodium hydroxide to separate the triethylamine and water into layers, thereby removing most of the water from the above-mentioned triethylamine;

[0007] 4. After phase separation, the crude triethylamine is distilled to remove water and obtain qualified triethylamine.

[0008] In step 3, the triethylamine obtained from steps 1 and 2 contains 10%-20% water. In the phase separator, the liquid is separated into an oil phase and an aqueous phase. The upper oil phase is triethylamine, and the lower aqueous phase is an alkaline solution. The water in the triethylamine reacts with excess caustic soda flakes. A discharge port is located at the bottom of the phase separator. Since the aqueous phase and excess caustic soda flakes are in the lower layer, they are usually discharged first. However, in the aqueous phase, the excess caustic soda flakes often absorb moisture and clump together, clogging the discharge port and affecting subsequent operations. Therefore, although it has the advantage of good dehydration effect on triethylamine, there is still considerable room for improvement. Utility Model Content

[0009] To facilitate the separation and discharge of the aqueous and oil phases in the phase separation tank, this application provides a triethylamine aqueous phase separation device.

[0010] The technical solution adopted in this application is as follows:

[0011] A triethylamine aqueous phase separation device includes a tank, a stirring element disposed in the tank, and an oil phase discharge pipe, an aqueous phase discharge pipe, and a drain pipe disposed at the bottom of the tank. The upper ends of the oil phase discharge pipe and the aqueous phase discharge pipe extend into the tank, with the upper end of the oil phase discharge pipe being higher than the upper end of the aqueous phase discharge pipe, and the upper end of the aqueous phase discharge pipe being higher than the upper end of the drain pipe. Each of the oil phase discharge pipe, the aqueous phase discharge pipe, and the drain pipe is equipped with an on / off valve.

[0012] By adopting the above technical solution, triethylamine is added to the tank, and caustic soda flakes are added to absorb the water in the triethylamine. After stirring for a period of time and allowing it to stand, the upper layer is the oil phase of triethylamine, and the lower layer is water. Some excess caustic soda flakes precipitate at the bottom of the tank. Therefore, during discharge, the water phase is first discharged through the water phase discharge pipe. When the oil phase appears in the components discharged from the water phase discharge pipe, it can be known that the boundary between the water and oil phases has reached the upper end of the water phase discharge pipe. Then, the material is discharged through the oil phase discharge pipe, which ensures that the material discharged from the oil phase discharge pipe is mainly the oil phase of triethylamine. Since both the oil phase discharge pipe and the water phase discharge pipe are higher than the drain pipe, the precipitated caustic soda flakes will not affect the discharge from the oil phase discharge pipe and the water phase discharge pipe.

[0013] Optionally, it also includes a connecting main pipe, the lower ends of the oil phase discharge pipe, the water phase discharge pipe and the sewage discharge pipe are all connected to the connecting main pipe, and the connecting main pipe is provided with an observation window.

[0014] By adopting the above technical solution, the discharge components can be better observed through the observation window to determine whether they are aqueous or oil phases, thus making a better judgment on the liquid level of the aqueous and oil phases.

[0015] Optionally, the upper end of the oil phase discharge pipe is 5-20 cm higher than the upper end of the water phase discharge pipe.

[0016] By adopting the above technical solution, the space in the tank can be better utilized, and the oil phase can be discharged more effectively.

[0017] Optionally, the impeller of the agitator is located between the upper end of the oil phase discharge pipe and the upper end of the water phase discharge pipe.

[0018] By adopting the above technical solution, the blade is located in a secondary position, which enables the caustic soda flakes to better adsorb moisture onto the oil phase, and makes it less likely for moisture to be carried into the oil phase during the standing process.

[0019] Optionally, a sealing element is provided in the oil phase discharge pipe, the sealing element being used to open and close one end of the oil phase discharge pipe located inside the tank.

[0020] By adopting the above technical solution, the upper end of the oil phase discharge pipe is sealed with a sealing component, thereby reducing the possibility of the water phase entering the oil phase discharge pipe during the stirring and settling process.

[0021] Optionally, the sealing component includes a connecting pipe that passes through the side wall of the oil phase discharge pipe and extends into the oil phase discharge pipe, and a sealing head that is slidably disposed in the connecting pipe. One end of the connecting pipe is used to connect to an external gas source. When the connecting pipe is in the gas supply state, the sealing head can seal one end of the oil phase discharge pipe in the tank.

[0022] By adopting the above technical solution, the plugging head can be sealed at the upper end of the oil phase discharge pipe when gas is supplied, thereby achieving the effect of sealing the oil phase discharge pipe. When the gas supply is stopped, the plugging head moves downward under the action of gravity, thereby opening the oil phase discharge pipe.

[0023] Optionally, the upper end of the oil phase discharge pipe has a structure that is larger at the top and smaller at the bottom, and the sealing head is located at the upper end of the oil phase discharge pipe, with a gap between it and the inner wall of the oil phase discharge pipe.

[0024] Optionally, the upper end of the oil phase discharge pipe is provided with discharge holes spaced apart, and the plug head is provided with a plug column. When the plug head moves upward, the plug column can be inserted into the discharge hole.

[0025] By adopting the above technical solution, the discharge hole can be better sealed by using a plugging column.

[0026] Optionally, the sealing head includes a connecting part slidably connected to the connecting pipe and a sealing part ball-hinged to the upper end of the connecting part. The plug is connected to the upper surface of the sealing part, and the plug is a frustum-shaped structure with a smaller upper part and a larger lower part. The discharge hole and the plug are adapted to each other.

[0027] By adopting the above technical solution, the sealing part can shake to a certain extent when the oil phase is discharged, which is more conducive to the discharge.

[0028] In summary, this application includes at least one of the following beneficial effects:

[0029] 1. The upper end of the oil phase discharge pipe is higher than the upper end of the water phase discharge pipe. Therefore, when the water phase discharge pipe discharges first, and the discharged material contains oil phase components, it can be known that the boundary between the water phase and the oil phase is close to the upper end of the water phase discharge pipe. The upper end of the oil phase discharge pipe is located in the oil phase. Therefore, the material discharged by the oil phase discharge pipe at this time is basically the oil phase.

[0030] 2. When it is necessary to clean the caustic soda flakes or other substances in the tank, simply open the drain outlet. Attached Figure Description

[0031] Figure 1 This is a schematic diagram of the structure of Embodiment 1 of this application;

[0032] Figure 2 This is a three-dimensional structural diagram of Embodiment 2 of this application;

[0033] Figure 3 This is a cross-sectional schematic diagram of the sealing component in Embodiment 2 of this application.

[0034] Explanation of reference numerals in the attached drawings: 1. Tank body; 2. Agitator; 3. Oil phase discharge pipe; 4. Water phase discharge pipe; 5. Sewage pipe; 6. Main connecting pipe; 7. Observation window; 8. Sealing component; 81. Connecting pipe; 82. Sealing head; 821. Connecting part; 822. Sealing part; 9. Discharge hole; 10. Plug; 11. First feed inlet; 12. Second feed inlet. Detailed Implementation

[0035] The present application will be further described in detail below with reference to the accompanying drawings.

[0036] Example 1

[0037] This application discloses a triethylamine water phase separation device. (Refer to...) Figure 1 The separation device includes a tank 1, an agitator 2 installed in the tank 1, and an oil phase discharge pipe 3, a water phase discharge pipe 4, and a sludge discharge pipe 5 installed at the lower end of the tank 1. The bottom of the tank 1 has an arc-shaped structure with the opening facing upwards. The sludge discharge pipe 5 is located at the center of the lower end of the tank 1, and one end of the sludge discharge pipe 5 is flush with the inner bottom surface of the tank 1, so that the sediment in the tank 1 can be discharged through the sludge discharge pipe 5. The oil phase discharge pipe 3, the water phase discharge pipe 4, and the sludge discharge pipe 5 are all equipped with on / off valves, which can be butterfly valves, ball valves, or other structures used in the prior art for controlling the opening and closing of the pipelines. The agitator 2 is a stirring shaft driven by a motor, and the lower side wall of the stirring shaft is provided with blades.

[0038] Both the aqueous phase discharge pipe 4 and the oil phase discharge pipe 3 extend into the tank body 1, with the upper end of the aqueous phase discharge pipe 4 higher than the upper opening of the drain pipe 5, and the upper end of the oil phase discharge pipe 3 higher than the upper end of the aqueous phase discharge pipe 4. In a further embodiment, the upper end of the oil phase discharge pipe 3 is 5-20 cm higher than the upper end of the aqueous phase discharge pipe 4, for example, 5 cm, 10 cm, or 15 cm. The impeller of the agitator 2 is located between the oil phase discharge pipe 3 and the aqueous phase discharge pipe 4.

[0039] The upper end of the tank 1 is provided with a cover, and the cover is provided with a first feed port 11 and a second feed port 12. The first feed port 11 is used to feed the triethylamine to be treated into the tank 1, and the second feed port 12 is used to add caustic soda flakes into the tank 1.

[0040] Triethylamine to be processed is added to tank 1 through the first inlet 11, and then a certain amount of caustic soda flakes are added to tank 1 through the second inlet 12. The agitator 2 is turned on, and after a period of reaction, the agitation is stopped, and the mixture is allowed to stand for a period of time, allowing the triethylamine and water to separate into two phases in tank 1. The upper oil phase is triethylamine, and the lower water phase is water. After standing, the water phase discharge pipe 4 is opened, allowing the water phase to be discharged, thus gradually shifting the interface between the water and oil phases downwards. When oil phase is discharged from the water phase discharge pipe 4, it indicates that the interface between the oil and water phases is near the upper end of the water phase discharge pipe 4. Discharge can continue through the water phase discharge pipe 4 for a while, and then discharge can continue through the oil phase discharge pipe 3, ensuring that the oil phase discharge pipe 3 almost entirely discharges oil-phase triethylamine. After the oil phase discharge pipe 3 is completely discharged, the remaining material in the pipe can be used for the next batch of triethylamine treatment, and caustic soda flakes can be added as needed. When tank 1 needs cleaning, the remaining material in tank 1 is cleaned and discharged through drain pipe 5. Therefore, the sediment in tank 1 will not affect the discharge of the aqueous and oil phases.

[0041] In a further embodiment, the lower ends of the oil phase discharge pipe 3, the water phase discharge pipe 4, and the sewage pipe 5 are connected to the same connecting main pipe 6. An observation window 7 is installed on the connecting main pipe 6. The observation window 7 is made of transparent material, which makes it easier to observe whether the outflowing material is water phase or oil phase.

[0042] The implementation principle of the triethylamine aqueous phase separation device in this application embodiment is as follows: Triethylamine to be processed is added to tank 1, and a certain amount of caustic soda flakes are added. The mixture is stirred by stirring element 2. After reacting for a period of time, it is allowed to stand and separate into layers. First, the material is discharged through aqueous phase discharge pipe 4. When the discharged material begins to contain oil phase, the discharge continues for a while. Then, the aqueous phase discharge pipe 4 is closed, and the material is discharged through oil phase discharge pipe 3. At this time, oil phase discharge pipe 3 is located above the interface between the oil phase and the aqueous phase, so the discharged material is basically oil phase.

[0043] Example 2

[0044] Reference Figure 2 and Figure 3 The difference between this embodiment and embodiment 1 is that a sealing element 8 for opening and closing the oil phase discharge pipe 3 is installed at the upper end of the oil phase discharge pipe 3. Under the action of the sealing element 8, the water phase is not easy to enter the oil phase discharge pipe 3 during the stirring or standing process.

[0045] The sealing component 8 includes a connecting pipe 81 that passes through the side wall of the oil phase discharge pipe 3 and extends into the oil phase discharge pipe 3, and a sealing head 82 that is slidably connected to the upper end of the connecting pipe 81. The upper end of the oil phase discharge pipe 3 has an open structure to allow liquid to flow through, and there is a gap between the connecting pipe 81 and the inner wall of the oil phase discharge pipe 3. One end of the connecting pipe 81 that extends out of the oil phase discharge pipe 3 is used to connect to a gas source, such as an air pump. When gas is supplied, the air pressure can drive the sealing head 82 to slide and seal the end of the oil phase discharge pipe 3. When discharge is required, the gas source is turned off, and the sealing head 82 can fall back into the connecting pipe 81 under the action of gravity.

[0046] Furthermore, the oil phase discharge pipe 3 has a structure that is wider at the top and narrower at the bottom at one end within the tank body 1. The plug head 82 is located within this structure, and there is a gap between the plug head 82 and the inner wall of the oil phase discharge pipe 3 to provide space for liquid to flow. The upper end of the oil phase discharge pipe 3 is provided with discharge holes 9 spaced apart, and a plug column 10 is fixed on the plug head 82 accordingly. When the plug head 82 moves upward, the plug column 10 can be inserted into the discharge hole 9, and the end of the plug column 10 can be flush with the end face of the oil phase discharge pipe 3.

[0047] The plugging head 82 includes a connecting part 821 that is slidably inserted into the connecting pipe 81 and a plugging part 822 that is ball-jointed to the upper end of the connecting part 821. A guide block and guide groove can be provided between the connecting part 821 and the oil phase discharge pipe 3, allowing the connecting part 821 to slide up and down in the oil phase discharge pipe 3 without rotating. The plug 10 is fixed to the upper surface of the plugging part 822, and the plug 10 has a frustum structure that is smaller at the top and larger at the bottom. The discharge hole 9 and the plug 10 are compatible, making it easier for the plug 10 to be inserted into the discharge hole 9. When the connecting part 821 moves downward, the plug 10 is not completely discharged from the discharge hole 9, making it easier to re-insert the plug 10 into the discharge hole 9. When the oil phase liquid is discharged, the plugging part 822 will experience some shaking, thereby promoting the discharge of the liquid.

[0048] The above are all preferred embodiments of this application, and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.

Claims

1. A triethylamine water phase separation device, characterized in that: It includes a tank body (1), a stirring component (2) installed in the tank body (1), and an oil phase discharge pipe (3), a water phase discharge pipe (4), and a sewage pipe (5) installed at the bottom of the tank body (1); the upper ends of the oil phase discharge pipe (3) and the water phase discharge pipe (4) extend into the tank body (1), and the upper end of the oil phase discharge pipe (3) is higher than the upper end of the water phase discharge pipe (4), the upper end of the water phase discharge pipe (4) is higher than the upper end of the sewage pipe (5), and an opening and closing valve is provided on the oil phase discharge pipe (3), the water phase discharge pipe (4), and the sewage pipe (5).

2. The triethylamine aqueous phase separation device according to claim 1, characterized in that: It also includes a connecting main pipe (6), the lower ends of the oil phase discharge pipe (3), the water phase discharge pipe (4) and the sewage pipe (5) are all connected to the connecting main pipe (6), and the connecting main pipe (6) is provided with an observation window (7).

3. The triethylamine aqueous phase separation device according to claim 2, characterized in that: The upper end of the oil phase discharge pipe (3) is 5-20cm higher than the upper end of the water phase discharge pipe (4).

4. The triethylamine aqueous phase separation device according to claim 3, characterized in that: The blades of the agitator (2) are located between the upper end of the oil phase discharge pipe (3) and the upper end of the water phase discharge pipe (4).

5. A triethylamine aqueous phase separation device according to any one of claims 1-4, characterized in that: A sealing element (8) is provided in the oil phase discharge pipe (3), and the sealing element (8) is used to open and close one end of the oil phase discharge pipe (3) located inside the tank body (1).

6. The triethylamine aqueous phase separation device according to claim 5, characterized in that: The sealing component (8) includes a connecting pipe (81) that passes through the side wall of the oil phase discharge pipe (3) and extends into the oil phase discharge pipe (3), and a sealing head (82) that is slidably disposed in the connecting pipe (81). One end of the connecting pipe (81) is used to connect to an external gas source. When the connecting pipe (81) is in the gas supply state, the sealing head (82) can seal one end of the oil phase discharge pipe (3) in the tank (1).

7. The triethylamine aqueous phase separation device according to claim 6, characterized in that: The upper end of the oil phase discharge pipe (3) has a structure that is larger at the top and smaller at the bottom. The sealing head (82) is located at the upper end of the oil phase discharge pipe (3) and there is a gap between it and the inner wall of the oil phase discharge pipe (3).

8. The triethylamine aqueous phase separation device according to claim 7, characterized in that: The upper end of the oil phase discharge pipe (3) is provided with discharge holes (9) spaced apart, and the plug head (82) is provided with a plug column (10). When the plug head (82) moves upward, the plug column (10) can be inserted into the discharge hole (9).

9. A triethylamine aqueous phase separation device according to claim 8, characterized in that: The sealing head (82) includes a connecting part (821) slidably connected to the connecting pipe (81) and a sealing part (822) ball-jointed to the upper end of the connecting part (821). The plug (10) is connected to the upper surface of the sealing part (822), and the plug (10) is a frustum-shaped structure with a smaller upper part and a larger lower part. The discharge hole (9) and the plug (10) are adapted to each other.

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