Butyl ester catalytic reaction and recovery system

Abstract

The utility model discloses a butyl ester catalytic reaction and recovery system, and belongs to the technical field of triisobutyl phosphate. According to the technical scheme, the device comprises a dropwise adding kettle, reaction kettles, a dealcoholization tower, a hydrochloric acid absorption tower, an alkaline washing tower, a water washing tower, a distillation tower, a butyl ester storage tank and a controller which are sequentially connected through pipelines, wherein the reaction kettles comprise the first reaction kettle and the second reaction kettle; the dropwise adding kettle is connected with an isobutanol storage tank through an isobutanol feeding pipeline, and an isobutanol feeding metering pump is arranged on the isobutanol feeding pipeline; the dropwise adding kettle is connected with a phosphorus oxychloride storage tank through a phosphorus oxychloride feeding pipeline, and a phosphorus oxychloride feeding metering pump is arranged on the phosphorus oxychloride feeding pipeline; the dropwise adding kettle is also connected with a catalyst feeding pipeline; and a catalyst feeding metering pump is arranged on the catalyst feeding pipeline. According to the utility model, the reaction sufficiency is promoted through the dripping kettle and the multi-stage reaction kettle, effective separation and purification of reaction products and byproducts are realized through stage-by-stage treatment, and the material recovery rate and the resource utilization rate are improved.

Description

Technical Field

[0001] The utility model belongs to the technical field of triisobutyl phosphate, and particularly relates to a butyl ester catalytic reaction and recovery system. Background Art

[0002] Triisobutyl phosphate (TBP), an important organophosphorus compound, is widely used in various fields due to its unique physical and chemical properties. As a plasticizer, it improves the flexibility and processing properties of plastics. As a defoamer, it effectively suppresses foaming in industries such as paints, coatings, and inks. Furthermore, as an extractant, TBP is widely used in the nuclear industry to extract elements such as uranium and plutonium due to its high selectivity for metal ions.

[0003] However, the traditional production process for triisobutyl phosphate faces numerous challenges. Optimizing parameters such as temperature, pressure, reaction time, and stirring can significantly improve reaction efficiency and product quality. However, the traditional process suffers from poor stirring in the reactor, leading to incomplete reactions and significant fluctuations in product quality. The "three wastes" generated during the production process—waste gas, waste liquid, and waste residue—are also pressing environmental challenges. In particular, the emission of volatile organic compounds (VOCs), such as hydrogen chloride gas and isobutanol, not only pollutes the environment but also increases environmental costs for companies. Utility Model Content

[0004] The utility model provides a butyl ester catalytic reaction and recovery system, which promotes the sufficiency of the reaction through a dropping kettle and a multi-stage reactor, and realizes effective separation and purification of reaction products and by-products through step-by-step treatment of a dealcoholization tower, a hydrochloric acid absorption tower, an alkali washing tower, a water washing tower and a distillation tower, thereby improving the material recovery rate and resource utilization rate.

[0005] The technical solution of the utility model is:

[0006] The butyl ester catalytic reaction and recovery system includes a dropping kettle, a reactor, a dealcoholization tower, a hydrochloric acid absorption tower, an alkali washing tower, a water washing tower, a distillation tower, a butyl ester storage tank and a controller, which are connected in sequence through pipelines. The reactor includes a reactor 1 and a reactor 2; the dropping kettle is connected to the isobutanol storage tank through an isobutanol feed pipeline, and an isobutanol feed metering pump is provided on the isobutanol feed pipeline; the dropping kettle is connected to the phosphorus oxychloride storage tank through a phosphorus oxychloride feed pipeline, and a phosphorus oxychloride feed meter is provided on the phosphorus oxychloride feed pipeline. The dropping kettle is also connected to a catalyst feed pipeline, a catalyst feed metering pump is provided on the catalyst feed pipeline, and the isobutanol feed metering pump, the phosphorus oxychloride feed metering pump and the catalyst feed metering pump are all electrically connected to the controller; the dropping kettle shell is provided with a cold brine feed pipeline and a cold brine discharge pipeline, and the cold brine feed pipeline and the cold brine discharge pipeline are both provided with a control valve 1, a temperature sensor 1 and a stirring device 1 are provided in the dropping kettle, and the control valve 1 and the temperature sensor 1 are both connected to the controller Electrical connection; Reactor 1 is provided with a heating jacket 1, Reactor 1 is provided with a temperature sensor 2 and a stirring device 2, and the temperature sensor 2 is electrically connected to the controller; Reactor 2 is provided with a heating jacket 2, Reactor 2 includes a Reactor 2 body and a motor 2, the upper end of the Reactor 2 body is open, a gas storage chamber is provided on the top of the Reactor 2 body, an air inlet valve is provided on one side of the air storage chamber, the Reactor 2 body is provided with a hollow stirring shaft and an exhaust valve, the upper end of the stirring shaft passes through the air storage chamber and is connected to Motor 2, a plurality of air inlet pipes are provided on the stirring shaft, all of which are located inside the air storage chamber, the hollow part of the stirring shaft is connected to the air storage chamber through the plurality of air inlet pipes, the lower end of the stirring shaft is provided with a stirring tube with closed ends, the stirring tube is provided with a plurality of jet nozzles, and the hollow part of the stirring shaft is connected to the plurality of jet nozzles through the stirring tube; Reactor 2 is provided with a temperature sensor 3, and the temperature sensor 3 is electrically connected to the controller; the dealcoholization tower is also connected to the dropping kettle through a pipeline; the hydrochloric acid absorption tower is connected to the smoke absorption pipeline.

[0007] Preferably, stirring device 1 and stirring device 2 both include a fixed frame and motor 1, the fixed frame is fixedly arranged on the dropping kettle or reactor 1, motor 1 is fixedly connected to the top of the fixed frame, the bottom end of motor 1 is fixedly connected to a rotating shaft and the rotating shaft is connected to a stirring paddle.

[0008] Preferably, the stirring shaft sleeve has an elastic sealing ring, the position of the elastic sealing ring relative to the stirring shaft is immovable, the top wall of the air storage chamber is provided with a groove, the elastic sealing ring is placed in the groove of the top wall of the air storage chamber, and is in a compressed state.

[0009] Preferably, the dropping kettle is provided with a pressure discharge port and a pressure sensor, and the pressure sensor is electrically connected to the controller.

[0010] Preferably, the smoke absorption pipeline is connected to an external vacuum unit.

[0011] Preferably, the top of the dealcoholization tower is connected to a top condenser, and the kettle of the dealcoholization tower is connected to a reboiler.

[0012] Compared with the prior art, the present invention has the following beneficial effects:

[0013] 1. This system incorporates metering pumps for isobutanol, phosphorus oxychloride, and the catalyst, electrically connected to a controller. This enables precise control and automated operation of reactant feeding. This helps reduce human error and improves the accuracy of reactant ratios, thereby enhancing reaction efficiency and product quality.

[0014] 2. The reaction is carried out in stages using Reactor 1 and Reactor 2. Temperature, stirring, and other conditions can be adjusted according to the reaction progress, optimizing the reaction path and further improving yield and product quality. The dropping reactor is equipped with a pressure relief port and pressure sensor, which are electrically connected to the controller. This allows for real-time monitoring and control of the pressure within the reactor, preventing overpressure accidents and enhancing system safety.

[0015] 3. The elastic sealing ring of the stirring shaft sleeve and its matching design with the groove on the top wall of the gas storage chamber effectively prevent gas leakage and further ensure production safety.

[0016] 4. The hydrochloric acid absorption tower and smoke absorption pipeline are connected to the external vacuum unit, which effectively absorbs the harmful gases generated during the reaction, reduces environmental pollution, and meets environmental protection requirements.

[0017] 5. Through the step-by-step treatment of dealcoholization tower, hydrochloric acid absorption tower, alkali washing tower, water washing tower and distillation tower, the reaction products and by-products are effectively separated and purified, and the material recovery rate and resource utilization rate are improved.

[0018] 6. Reactor 2 adopts a stirring method that combines gas stirring and mechanical structure stirring, which greatly improves the stirring efficiency, enables the reaction liquid to be mixed more fully, and greatly improves the production reaction efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is a structural diagram of the present utility model.

[0020] Figure 2 It is a structural diagram of a reactor 1 of the present invention.

[0021] Figure 3 It is a structural diagram of the reactor 2 of the present utility model.

[0022] In the figure, 1. Dropping kettle; 101. Isobutanol feed line; 102. Phosphorus oxychloride feed line; 103. Catalyst feed line; 104. Cold brine feed line; 105. Cold brine discharge line; 2. Dealcoholization tower; 201. Top condenser; 202. Reboiler; 3. Hydrochloric acid absorption tower; 4. Alkali washing tower; 5. Water washing tower; 6. Distillation tower; 7. Butyl ester storage tank; 8. Reactor 1; 9. Reactor 2; 901. Motor 2; 902. Gas storage chamber; 903. Inlet valve; 904. Stirring shaft; 905. Exhaust valve; 906. Inlet pipe; 907. Stirring tube; 908. Injector head; 10. Isobutanol storage tank; 11. Phosphorus oxychloride storage tank; 13. Fixed frame; 14. Motor 1; 15. Rotating shaft; 16. Stirring paddle. DETAILED DESCRIPTION

[0023] In order to enable those skilled in the art to better understand the technical solutions of the present invention, the following will be combined with the drawings of the embodiments of the present invention to clearly and completely describe the technical solutions of the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts should fall within the scope of protection of the present invention.

[0024] Example 1

[0025] like Figure 1-3 As shown, this embodiment provides a butyl ester catalytic reaction and recovery system, including a dropping kettle 1, a reactor, a dealcoholization tower 2, a hydrochloric acid absorption tower 3, an alkali washing tower 4, a water washing tower 5, a distillation tower 6, a butyl ester storage tank 7 and a controller connected in sequence by pipelines, the reactors include a reactor 1 8 and a reactor 2 9; the top of the dealcoholization tower 2 is connected to a tower top condenser 201, and the reactor of the dealcoholization tower 2 is connected to a reboiler 202.

[0026] The dropping kettle 1 is connected to the isobutanol storage tank 10 through the isobutanol feed line 101, and the isobutanol feed line 101 is provided with an isobutanol feed metering pump; the dropping kettle 1 is connected to the phosphorus oxychloride storage tank 11 through the phosphorus oxychloride feed line 102, and the phosphorus oxychloride feed line 102 is provided with a phosphorus oxychloride feed metering pump; the dropping kettle 1 is also connected to the catalyst feed line 103, and the catalyst feed line 103 is provided with a catalyst feed metering pump, and the isobutanol feed metering pump, the phosphorus oxychloride feed metering pump and the catalyst feed metering pump are all electrically connected to the controller; the dropping kettle 1 is provided with a pressure discharge port and a pressure sensor, and the pressure sensor is electrically connected to the controller;

[0027] The shell of the dropping kettle 1 is provided with a cold brine feed pipeline 104 and a cold brine discharge pipeline 105, and the cold brine feed pipeline 104 and the cold brine discharge pipeline 105 are both provided with a control valve 1. A temperature sensor 1 and a stirring device 1 are provided in the dropping kettle 1, and the control valve 1 and the temperature sensor 1 are both electrically connected to the controller;

[0028] Reactor 1 8 is provided with a heating jacket 1, and a temperature sensor 2 and a stirring device 2 are provided inside the reactor 1 8. The temperature sensor 2 and the control switch of the heating jacket 1 are electrically connected to the controller; the stirring device 1 and the stirring device 2 each include a fixed frame 13 and a motor 14. The fixed frame 13 is fixedly arranged on the dropping kettle 1 or the reactor 1 8. The motor 14 is fixedly connected to the top of the fixed frame 13. The bottom end of the motor 14 is fixedly connected to a rotating shaft 15, and the rotating shaft 15 is connected to a stirring paddle 16.

[0029] Reactor 2 9 is provided with a heating jacket 2, and reactor 2 9 includes a reactor 2 body and a motor 2 901. The upper end of the reactor 2 body is open, and the top of the reactor 2 body is provided with an air storage chamber 902, and an air inlet valve 903 is provided on one side of the air storage chamber 902. The reactor 2 body is provided with a stirring shaft 904 and an exhaust valve 905 with a hollow structure. The upper end of the stirring shaft 904 passes through the air storage chamber 902 and is connected to the motor 2 901. A plurality of air inlet pipes 906 are provided on the stirring shaft 904, all of which are located inside the air storage chamber 902. The hollow structure of the stirring shaft 904 The stirring shaft 904 is connected to the air storage chamber 902 through multiple air inlet pipes 906. The lower end of the stirring shaft 904 is provided with a stirring tube 907 with closed ends. The stirring tube 907 is provided with multiple air nozzles 908. The hollow part of the stirring shaft 904 is connected to the multiple air nozzles 908 through the stirring tube 907; the stirring shaft 904 is covered with an elastic sealing ring, and the position of the elastic sealing ring relative to the stirring shaft cannot be moved. The top wall of the air storage chamber 902 is provided with a groove. The elastic sealing ring is placed in the groove of the top wall of the air storage chamber and is in a compressed state.

[0030] Reactor 2 9 is provided with temperature sensor 3, which is electrically connected to the controller; dealcoholization tower 2 is also connected to dropping kettle 1 through a pipeline; hydrochloric acid absorption tower 3 is connected to a smoke absorption pipeline, which is connected to an external vacuum unit.

[0031] Based on preset parameters, the controller activates the isobutanol feed metering pump and the catalyst feed metering pump, accurately metering the isobutanol and catalyst into the stirring device within the dropping kettle 1. Motor 14 drives the stirring paddle 16, which then begins to operate, thoroughly mixing the materials. Simultaneously, cold brine enters the shell of the dropping kettle 1 through the cold brine feed line 104 for circulating cooling, maintaining the reaction temperature at 10°C. Phosphorus oxychloride is continuously added to the dropping kettle 1 through the dropping line, and the cooled brine is discharged through the cold brine discharge line 105. Control valve 1 adjusts the flow rate of the cold brine based on feedback from temperature sensor 1.

[0032] The evenly mixed materials enter the reactor 1 8 through the pipeline. The heating jacket is initially heated to 20°C. At the same time, the stirring device 2 works to further promote the reaction. The reaction time is 5 hours. The temperature sensor 2 monitors the temperature in the reactor 1 in real time and feeds the data back to the controller. The controller adjusts the heating power of the heating jacket 1 according to the set temperature.

[0033] After the initial reaction, the materials enter Reactor 2 9 . Heating jacket 2 begins heating, maintaining the reaction temperature at 35°C. Motor 2 901 drives the stirring shaft 904 of Reactor 2 9 . Simultaneously, gas within gas storage chamber 902 enters the hollow portion of stirring shaft 904 through gas inlet pipe 906 and is then ejected through nozzle 908 on stirring tube 907 , creating a uniform bubble distribution and promoting gas-liquid mass transfer and reaction. Temperature sensor 3 monitors the temperature within Reactor 2 to ensure the reaction proceeds at optimal temperature conditions. After the reaction is complete, the materials first enter dealcoholization tower 2 for dealcoholization. The overhead condenser 201 condenses and recovers the alcohol byproduct, while the tower reboiler 202 maintains the tower temperature. Some unreacted isobutanol can be returned to the addition tank 1 via a pipeline for further processing. The dealcoholized materials then enter hydrochloric acid absorption tower 3 (to absorb acidic gases), alkali scrubber 4 (to neutralize residual acidic substances), and water scrubber 5 (to remove impurities) for purification. The purified material enters the distillation tower 6 for distillation and purification, and finally obtains a high-purity butyl ester product, which is stored in the butyl ester storage tank 7.

[0034] The harmful gases generated during the reaction are absorbed and treated by an external vacuum unit through a smoke absorption pipeline to prevent environmental pollution. The dropping kettle 1 is equipped with a pressure relief port and a pressure sensor to monitor the pressure inside the kettle in real time to prevent overpressure accidents.

[0035] Although the present invention has been described in detail with reference to the accompanying drawings and in conjunction with preferred embodiments, the present invention is not limited thereto. Without departing from the spirit and substance of the present invention, persons of ordinary skill in the art may make various equivalent modifications or substitutions to the embodiments of the present invention, and such modifications or substitutions shall fall within the scope of the present invention. Therefore, the scope of protection of the present invention shall be subject to the scope of protection of the claims.

Claims

1. A butyl ester catalytic reaction and recovery system, comprising a dropping kettle (1), a reaction kettle, a dealcoholization tower (2), a hydrochloric acid absorption tower (3), an alkali washing tower (4), a water washing tower (5), a distillation tower (6), a butyl ester storage tank (7), and a controller, which are sequentially connected through pipelines, and is characterized in that; The reactor includes reactor 1 (8) and reactor 2 (9); The dropping kettle (1) is connected to the isobutanol storage tank (10) via the isobutanol feed pipeline (101), and the isobutanol feed metering pump is provided on the isobutanol feed pipeline (101); the dropping kettle (1) is connected to the phosphorus oxychloride storage tank (11) via the phosphorus oxychloride feed pipeline (102), and the phosphorus oxychloride feed metering pump is provided on the phosphorus oxychloride feed pipeline (102); the dropping kettle (1) is also connected to the catalyst feed pipeline (103), and the catalyst feed metering pump is provided on the catalyst feed pipeline (103); the isobutanol feed metering pump, the phosphorus oxychloride feed metering pump and the catalyst feed metering pump are all electrically connected to the controller; The shell of the dropping kettle (1) is provided with a cold brine feed pipeline (104) and a cold brine discharge pipeline (105), and the cold brine feed pipeline (104) and the cold brine discharge pipeline (105) are both provided with a control valve 1. A temperature sensor 1 and a stirring device 1 are provided in the dropping kettle (1), and the control valve 1 and the temperature sensor 1 are both electrically connected to the controller; Reactor 1 (8) is provided with a heating jacket 1, and temperature sensor 2 and stirring device 2 are provided inside reactor 1 (8), and temperature sensor 2 is electrically connected to the controller; Reactor 2 (9) is provided with a heating jacket 2. Reactor 2 (9) includes a reactor 2 body and a motor 2 (901). The upper end of the reactor 2 body is open. The top of the reactor 2 body is provided with a gas storage chamber (902). One side of the gas storage chamber (902) is provided with an air inlet valve (903). The reactor 2 body is provided with a hollow stirring shaft (904) and an exhaust valve (905). The upper end of the stirring shaft (904) passes through the gas storage chamber (902) and is connected to the motor 2 (901). The stirring shaft (904) is provided with a plurality of air inlet pipes (906) all located inside the air storage chamber (902); the hollow portion of the stirring shaft (904) is communicated with the air storage chamber (902) via the plurality of air inlet pipes (906); the lower end of the stirring shaft (904) is provided with a stirring tube (907) with closed ends; the stirring tube (907) is provided with a plurality of air jets (908); the hollow portion of the stirring shaft (904) is communicated with the plurality of air jets (908) via the stirring tube (907); A temperature sensor 3 is provided in the reactor 2 (9), and the temperature sensor 3 is electrically connected to the controller; The dealcoholization tower (2) is also connected to the dropping kettle (1) through a pipeline; The hydrochloric acid absorption tower (3) is connected to a smoke absorption pipeline.

2. The butyl ester catalytic reaction and recovery system according to claim 1, characterized in that: The stirring device 1 and the stirring device 2 both comprise a fixed frame (13) and a motor 1 (14). The fixed frame (13) is fixedly arranged on the dropping kettle (1) or the reactor 1 (8). The motor 1 (14) is fixedly connected to the top of the fixed frame (13). The bottom end of the motor 1 (14) is fixedly connected to a rotating shaft (15), and the rotating shaft (15) is connected to a stirring paddle (16).

3. The butyl ester catalytic reaction and recovery system according to claim 1, characterized in that: The stirring shaft (904) is sleeved with an elastic sealing ring, and the position of the elastic sealing ring relative to the stirring shaft cannot be moved. The top wall of the air storage chamber (902) is provided with a groove, and the elastic sealing ring is placed in the groove of the top wall of the air storage chamber (902) and is in a compressed state.

4. The butyl ester catalytic reaction and recovery system according to claim 1, characterized in that: The dropping kettle (1) is provided with a pressure discharge port and a pressure sensor, and the pressure sensor is electrically connected to the controller.

5. The butyl ester catalytic reaction and recovery system according to claim 1, characterized in that: The smoke absorption pipeline is connected to the external vacuum unit.

6. The butyl ester catalytic reaction and recovery system according to claim 1, characterized in that: The top of the dealcoholization tower (2) is connected to a top condenser (201), and the bottom of the dealcoholization tower (2) is connected to a reboiler (202).

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