Continuous separation device for mixture of petroleum ether and phosphorus trichloride
By designing a continuous separation device including mixing tubes and phase separation tanks, using hydrolysis reaction and phase separation technology, the problem of ineffective separation of petroleum ether and phosphorus trichloride mixture is solved, and efficient resource utilization and environmental protection are achieved. .
Patent Information
- Application Number
- CN202420910648.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-29
- Publication Date
- 2025-02-25
- Estimated Expiration
- 2034-04-29
AI Technical Summary
In the production process of synthesis of methyl phosphorus dichloride by aluminum method, the mixture of petroleum ether and phosphorus trichloride cannot be effectively separated by distillation or rectification, resulting in waste of resources, increased production costs and environmental pollution.
Design a continuous separation device, including a mixing tube and a phase separation tank, and realizes petroleum ether and trichloride by hydrolyzing phosphorus trichloride and water in the mixing tube, and separates the light and heavy components using a phase separation tank to achieve petroleum ether and trichlorogenic Separation of phosphorus chloride.
The continuous separation of petroleum ether and phosphorus trichloride is achieved, and the reuse of petroleum ether can be recovered as a solvent. The aqueous phosphorite solution has multiple uses, reducing resource waste and environmental pollution and improving production efficiency.
Smart Images
Figure CN222518608U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of production of methyl phosphorus dichloride synthesized by aluminum process, in particular to a continuous separation device of a mixture of petroleum ether and phosphorus trichloride. Background Art
[0002] In the production process of synthesizing methyl phosphorus dichloride by aluminum method, aluminum powder is used as raw material, and reacts with chloromethane to obtain methyl aluminum sesquichloride, which then reacts with aluminum trichloride to obtain methyl aluminum dichloride, which then reacts with phosphorus trichloride to obtain a complex, and finally, after dissociation of substances such as alkali metal salts, methyl phosphorus dichloride is obtained; the reaction of methyl aluminum dichloride and phosphorus trichloride is a violent exothermic process. For safety reasons, petroleum ether or phosphorus trichloride or a mixture of the two is often used as a reaction solvent in the process to dilute the material and remove the heat generated by the reaction in time to ensure that the process parameters are within the normal range. In the process using petroleum ether, a mixture of petroleum ether and phosphorus trichloride will appear (the mass ratio of the two is about 5~10:1). Since the boiling point range of petroleum ether is large, the boiling point of phosphorus trichloride is 74%~78℃, which is just within the boiling range of petroleum ether, and it cannot be effectively separated by distillation or rectification.
[0003] If the petroleum ether and phosphorus trichloride in the mixture cannot be effectively separated, then the two substances cannot be fully utilized. This not only wastes precious raw material resources, but also increases production costs and reduces economic benefits. The mixture of petroleum ether and phosphorus trichloride that cannot be effectively separated may cause environmental pollution during the treatment process. Once these chemicals leak into the soil, water or air, they may have a long-term impact on the ecosystem. However, there is currently no effective separation method or device to separate petroleum ether from phosphorus trichloride. Utility Model Content
[0004] Aiming at the problem that petroleum ether and phosphorus trichloride cannot be effectively separated, the utility model provides a device for continuously quenching and phase-separating to treat the petroleum ether-phosphorus trichloride mixture.
[0005] In order to achieve the above-mentioned invention object, the technical solution of the utility model is as follows:
[0006] A continuous separation device for a mixture of petroleum ether and phosphorus trichloride, comprising a mixing tube and a phase separation tank, wherein the mixing tube is a hollow structure, one side of the mixing tube is provided with two feed ports, wherein the first feed port of the mixing tube is a water feed port, and the second feed port of the mixing tube is a feed port of a petroleum ether-phosphorus trichloride mixture; the other side of the mixing tube is provided with a discharge port; the phase separation tank is a hollow structure, one side of the phase separation tank is provided with a phase separation tank feed port, the phase separation tank feed port is connected to the mixing tube discharge port, and the bottom of the phase separation tank is close to the phase separation tank feed port. A heavy component outlet is provided on one side of the phase separation tank outlet, a light component outlet is provided on the bottom of the phase separation tank away from the phase separation tank feed port, a vertically upward baffle is provided between the heavy component outlet and the light component outlet, the baffle is fixedly connected to the bottom of the tank body, a space is left between the baffle and the top of the tank body, a cooling device is provided on the outer surface of the mixing tube; the cooling device is a mixing tube jacket, a coolant inlet is provided on the bottom of the jacket close to the mixing tube discharge port, and a coolant outlet is provided on the top of the jacket close to the mixing tube feed port.
[0007] A static mixer is arranged in the hollow interior of the mixing tube.
[0008] A cooling device is arranged on the outer surface of the mixing tube, and the cooling device is a mixing tube jacket. A coolant inlet is arranged at the bottom of the jacket near the mixing tube discharge port, and a coolant outlet is arranged at the top of the jacket near the mixing tube feed port.
[0009] The heavy component outlet of the phase separation tank is provided with a downward protrusion, which prolongs the phase separation time of the mixed liquid and achieves a better phase separation effect, so that the heavy component outlet position extends downward, avoiding the light component from being mixed with the heavy component at the bottom due to incomplete separation and being discharged from the heavy component outlet.
[0010] A tail gas interface is provided on the top of the phase separation tank, and the tail gas generated in the phase separation tank is discharged through the tail gas interface.
[0011] A temperature detector is arranged in the mixing tube to monitor the reaction temperature in the mixing tube.
[0012] The mixing tube feed port, the coolant feed port, the phase separation tank feed port, the mixing tube discharge port, the phase separation tank heavy component outlet and the light component outlet are respectively provided with automatic control valves.
[0013] The mixing tube feed port, the coolant feed port and the phase separation tank feed port are also respectively provided with flow meters, and the feed amount of each feed port is monitored by the flow meters, so as to adjust the automatic control valve.
[0014] The second mixing tube feed port is provided with a density meter, which monitors the density change of the petroleum ether-phosphorus trichloride mixture in real time to monitor the ratio of petroleum ether to phosphorus trichloride, and changes the feed amount of water in the mixture according to different ratios, thereby controlling the ratio of phosphorus trichloride to water, thereby ensuring that the phosphorus trichloride can fully react.
[0015] An interface level meter is arranged in the phase separation tank, and the interface level meter monitors the height of the phase separation interface between the aqueous solution and the petroleum ether in real time. When the interface is too high, the valves at the feed inlet of the phase separation tank and the light component outlet are closed, and the automatic control valve at the heavy component outlet is opened; when the interface is too low, the valves at the feed inlet of the phase separation tank and the heavy component outlet are closed, and the automatic control valve at the light component outlet is opened.
[0016] The continuous separation device also includes a PLC controller, and the temperature detector, automatic control valve, flow meter, density meter and interface liquid level meter are electrically connected to the PLC controller respectively.
[0017] Beneficial effects of the utility model:
[0018] 1. In the utility model, deionized water is introduced at a certain speed from a feed port of a mixing tube, and then the coolant outlet and the coolant inlet of the mixing tube are opened. After the temperature of the material in the reactor is reduced to a specified temperature, a petroleum ether-phosphorus trichloride mixture is introduced at a certain flow rate from another feed port of the mixing tube. Phosphorus trichloride is hydrolyzed with water in the mixing tube to generate phosphorous acid. The material after the reaction in the mixing reactor directly enters a phase separation tank, and the light and heavy components are separated after phase separation, wherein the light component is petroleum ether, and the heavy component is a phosphorous acid aqueous solution.
[0019] 2. In the utility model, the separated petroleum ether can be directly recovered and reused as a solvent to save resources; the recovered phosphorous acid aqueous solution has multiple uses. First, the recovered phosphorous acid aqueous solution can be used as a chemical raw material. In chemical production, it can be used as an important raw material for synthesizing other compounds, participating in various chemical reactions, and preparing the required chemicals. Secondly, the phosphorous acid aqueous solution also has certain applications in the medical field. It can be used as a synthetic raw material or additive for certain drugs and used in the pharmaceutical process. In addition, the recovered phosphorous acid aqueous solution can also be used for metal surface treatment as an anticorrosive agent or surface treatment agent to improve the corrosion resistance of metals or improve their surface properties.
[0020] 3. In the utility model, the material after the reaction in the mixing reactor is a mixture of an aqueous phosphorous acid solution and petroleum ether. Since the aqueous phosphorous acid solution and petroleum ether are immiscible with each other, the mixture of the aqueous phosphorous acid solution and the petroleum ether is stratified in a separation tank, wherein the petroleum ether as a light component overflows in the upper layer and flows out through the upper part of the baffle through the light component outlet, while the aqueous phosphorous acid solution as a heavy component is blocked by the baffle in the lower layer and flows out through the heavy component outlet.
[0021] 4. The utility model has reasonable design, simple structure and convenient operation. The phosphorus trichloride in the phosphorus chloride mixture reacts with water in a mixing tube to form a phosphorous acid solution, and then the light and heavy components are separated in a separation tank to achieve separation of petroleum ether and phosphorus trichloride. The utility model can achieve continuous separation of petroleum ether and phosphorus trichloride mixture without interrupting the production process or manual operation, effectively reducing the workload of operators and achieving good separation effect. BRIEF DESCRIPTION OF THE DRAWINGS
[0022] Figure 1 The utility model is a schematic diagram of the structure of a continuous separation device for a mixture of petroleum ether and phosphorus trichloride.
[0023] Among them, 1. Mixing tube feed port 1; 2. Mixing tube feed port 2; 3. Coolant outlet; 4. Coolant inlet; 5. Mixing tube; 6. Phase separation tank; 7. Heavy component outlet; 8. Light component outlet; 9. Mixing tube discharge port; 10. Phase separation tank feed port; 11. Baffle. DETAILED DESCRIPTION
[0024] The present invention is further described in detail below in conjunction with the embodiments, but the implementation manner of the present invention is not limited thereto.
[0025] Example 1
[0026] This embodiment provides a Figure 1 The continuous separation device of the mixture of petroleum ether and phosphorus trichloride shown in the figure comprises a mixing tube 5 and a phase separation tank 6, wherein the mixing tube 5 is a hollow structure, and a static mixer is arranged in the hollow interior of the mixing tube 5; two feed ports are arranged on one side of the mixing tube 5, wherein the mixing tube feed port 1 is a water feed port, and the mixing tube feed port 2 is a petroleum ether-phosphorus trichloride mixture feed port; a discharge port is arranged on the other side of the mixing tube 5; the phase separation tank 6 is a hollow structure, and a phase separation tank feed port 10 is arranged on one side of the phase separation tank 6, and the phase separation tank feed port 10 is connected to the mixing tube discharge port 9, and a heavy component is arranged on the side of the bottom of the phase separation tank 6 near the phase separation tank feed port 10. Outlet 7, a light component outlet 8 is arranged on the side of the bottom of the phase separation tank 6 away from the phase separation tank feed port 10, a vertical upward baffle 11 is arranged between the heavy component outlet 7 and the light component outlet 8, the baffle 11 is fixedly connected to the bottom of the tank body, and a space is left between the baffle 11 and the top of the tank body; a cooling device is arranged on the outer surface of the mixing tube 5; the cooling device is a mixing tube jacket, and a coolant inlet 4 is arranged on the bottom of the jacket near the mixing tube discharge port 9, and a coolant outlet 3 is arranged on the top of the jacket near the mixing tube feed port 1; a downward protrusion is arranged at the heavy component outlet 7 of the phase separation tank 6; an exhaust gas interface is arranged on the top of the phase separation tank 6.
[0027] In this embodiment, deionized water is introduced at a certain speed from a feed port of the mixing tube 5, and then the coolant outlet 3 and the inlet of the mixing tube 5 are opened. After the temperature of the material in the reactor is reduced to a specified temperature, a petroleum ether-phosphorus trichloride mixture is introduced at a certain flow rate from another feed port of the mixing tube. The phosphorus trichloride is hydrolyzed with water in the mixing tube 5 to generate phosphorous acid. The material after the reaction in the mixing reactor directly enters the phase separation tank 6. The material after the reaction in the mixing reactor is a mixture of phosphorous acid aqueous solution and petroleum ether. Since phosphorous acid aqueous solution and petroleum ether are immiscible with each other, the mixture of phosphorous acid aqueous solution and petroleum ether is stratified in the separation tank, wherein the petroleum ether of the light component overflows in the upper layer through the upper part of the baffle 11 and flows out through the light component outlet 8, while the phosphorous acid aqueous solution of the heavy component is blocked by the baffle 11 in the lower layer and flows out through the heavy component outlet 7.
[0028] In the utility model, a static mixer is arranged in the mixing tube 5, so that the petroleum ether-phosphorus trichloride mixture fluid and the water fluid are cut, sheared, rotated and remixed, so as to achieve the purpose of good dispersion and sufficient mixing between the fluids; the protrusions are arranged to extend the phase separation time of the mixed liquid, so as to achieve a better phase separation effect, so that the position of the heavy component outlet 7 is extended downward, so as to avoid the light component from being mixed with the heavy component at the bottom due to incomplete separation and being discharged from the heavy component outlet 7; and an exhaust gas interface is arranged on the top of the phase separation tank 6, through which the exhaust gas generated in the phase separation tank 6 is discharged.
[0029] Example 2
[0030] Compared with Example 1, the present embodiment is different in that, in the present embodiment, a temperature detector is arranged in the mixing tube 5; the mixing tube feed port, the coolant feed port, the phase separation tank feed port 10, the mixing tube discharge port 9, the phase separation tank heavy component outlet 7 and the light component outlet 8 are respectively provided with automatic control valves; the mixing tube feed port, the coolant feed port and the phase separation tank feed port 10 are also respectively provided with flow meters; the mixing tube feed port 2 is provided with a density meter; the phase separation tank 6 is provided with an interface liquid level meter; the continuous separation device also includes a PLC controller, and the temperature detector, automatic control valve, flow meter, density meter and interface liquid level meter are respectively electrically connected to the PLC controller.
[0031] In this embodiment, the PLC controller monitors the ratio of petroleum ether to phosphorus trichloride in the petroleum ether-phosphorus trichloride mixture through the density meter at the mixing tube feed port 2 to control the water feed amount. The temperature sensor in the mixing tube 5 monitors the temperature in the mixing tube 5 in real time. The PLC controller adjusts the automatic control valve of the coolant inlet and outlet according to the data of the temperature sensor in the mixing tube 5 to control the temperature in the mixing tube 5. After the phosphorus trichloride in the mixture reacts with water, it is introduced into the phase separation tank 6. After phase separation in the phase separation tank 6, the aqueous solution and petroleum ether are discharged from the heavy component outlet 7 and the light component outlet 8 respectively. The interface level meter monitors the phase separation interface height of the aqueous solution and petroleum ether in real time. When the interface is too high, the valves at the phase separation tank feed port 10 and the light component outlet 8 are closed, and the automatic control valve of the heavy component outlet 7 is opened; when the interface is too low, the valves at the phase separation tank feed port 10 and the heavy component outlet 7 are closed, and the automatic control valve of the light component outlet 8 is opened;
[0032] In this embodiment, a flow meter is provided at each material inlet, and the flow rate of each feed port is monitored in real time by the flow meter and transmitted to the PLC processor. The PLC processor controls the automatic control valve at each material inlet according to the data of the temperature sensor, the density meter and the interface liquid level meter to adjust the feed amount; when the temperature in the mixing tube 5 rises abnormally, the automatic control valve at the mixing tube feed port is urgently cut off to prevent the temperature from further rising.
[0033] It is understood that the present invention is described by some embodiments, and those skilled in the art are aware that various changes or equivalent substitutions may be made to these features and embodiments without departing from the spirit and scope of the present invention. In addition, under the teachings of the present invention, these features and embodiments may be modified to adapt to specific circumstances and materials without departing from the spirit and scope of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed herein, and all embodiments falling within the scope of the claims of this application are within the scope of protection of the present invention.
Claims
1. A continuous separation device for a mixture of petroleum ether and phosphorus trichloride, characterized in that: The invention comprises a mixing tube (5) and a phase separation tank (6), wherein the mixing tube (5) is a hollow structure, and one side of the mixing tube (5) is provided with two feed ports, wherein the first mixing tube feed port (1) is a water feed port, and the second mixing tube feed port (2) is a petroleum ether-phosphorus trichloride mixture feed port; the other side of the mixing tube (5) is provided with a discharge port; the phase separation tank (6) is a hollow structure, and one side of the phase separation tank (6) is provided with a phase separation tank feed port (10), wherein the phase separation tank feed port (10) is connected to the mixing tube discharge port (9), and a heavy component outlet (10) is provided at the bottom of the phase separation tank (6) near the phase separation tank feed port (10). 7), a light component outlet (8) is provided at the bottom of the phase separation tank (6) on the side away from the phase separation tank feed port (10), a baffle (11) vertically upward is provided between the heavy component outlet (7) and the light component outlet (8), the baffle (11) is fixedly connected to the bottom of the tank body, and a space is left between the baffle (11) and the top of the tank body, and a cooling device is provided on the outer surface of the mixing tube (5); the cooling device is a mixing tube (5) jacket, and a cooling liquid inlet (4) is provided at the bottom of the jacket near the mixing tube discharge port (9), and a cooling liquid outlet (3) is provided at the top of the jacket near the mixing tube feed port (1).
2. The continuous separation device of the mixture of petroleum ether and phosphorus trichloride according to claim 1, characterized in that: A static mixer is arranged in the hollow interior of the mixing tube (5).
3. The continuous separation device of the mixture of petroleum ether and phosphorus trichloride according to claim 1, characterized in that: A downward protrusion is provided at the heavy component outlet (7) of the phase separation tank.
4. The continuous separation device of the mixture of petroleum ether and phosphorus trichloride according to claim 1, characterized in that: The top of the phase separation tank (6) is provided with an exhaust gas interface.
5. The continuous separation device of the mixture of petroleum ether and phosphorus trichloride according to claim 1, characterized in that: The mixing tube (5) is provided with a temperature detector for monitoring the reaction temperature in the mixing tube (5).
6. The continuous separation device of the mixture of petroleum ether and phosphorus trichloride according to claim 1, characterized in that: The mixing tube feed port, the coolant feed port, the phase separation tank feed port (10), the mixing tube discharge port (9), the phase separation tank heavy component outlet (7) and the light component outlet (8) are respectively provided with automatic control valves; the mixing tube feed port, the coolant feed port and the phase separation tank feed port (10) are also respectively provided with flow meters.
7. The continuous separation device of the mixture of petroleum ether and phosphorus trichloride according to claim 1, characterized in that: The mixing tube feed port 2 (2) is provided with a density meter.
8. The continuous separation device of the mixture of petroleum ether and phosphorus trichloride according to claim 1, characterized in that: An interface liquid level meter is arranged in the phase separation tank (6).
9. The continuous separation device of the mixture of petroleum ether and phosphorus trichloride according to claim 1, characterized in that: The continuous separation device also includes a PLC controller.
10. The continuous separation device of the mixture of petroleum ether and phosphorus trichloride according to claim 9, characterized in that: The PLC controller is electrically connected to the temperature detector, the automatic control valve, the flow meter, the density meter and the interface liquid level meter respectively.