Integrated carbon tetrachloride rectification impurity removal device

Abstract

The utility model discloses an integrated carbon tetrachloride rectification and impurity removal device, including rectifying column, reflux tank, alkali washing layered jar and azeotrope tower, bottom and top are equipped with first discharge gate, second discharge gate, and the second discharge gate is connected with the overhead condenser through the pipeline, and one side of reflux tank is connected through the pipeline, and one end of reflux tank is connected with reflux pump, and the tail end of reflux pump is connected to the top of rectifying column, the bottom of reflux tank is equipped with double -path condenser, and the top of double -path condenser is connected with first condensing pipe and second condensing pipe, and the other end of second condensing pipe is connected with reflux tank, and the top of first condensing pipe and azeotrope tower is connected through the pipeline, the bottom side of alkali washing layered jar is equipped with azeotrope pipeline, and the tail end of azeotrope pipeline is connected in the bottom side of azeotrope tower. The integrated design of rectifying column, reflux tank, alkali washing layered jar and azeotrope tower of the design, discarded the complicated multi -device and pipeline connection, saved the equipment space, reduced the manufacturing cost.

Description

Technical Field

[0001] This utility model relates to the field of carbon tetrachloride distillation technology, and in particular to an integrated carbon tetrachloride distillation and impurity removal device. Background Technology

[0002] Currently, 3%-5% of carbon tetrachloride is generated during the production of methane chloride. The application of carbon tetrachloride as a chemical raw material in the production of non-ODS substances (ODS: ozone-depleting substances) is unrestricted. Therefore, using carbon tetrachloride as a raw material to prepare other chemicals has become a new way to convert excess carbon tetrachloride.

[0003] However, the purity of carbon tetrachloride after distillation is currently not high, and it contains impurities such as chloroform, which further affect the purity of carbon tetrachloride and limit its application. Furthermore, traditional carbon tetrachloride distillation technology typically employs a continuous "two-tower" or "three-tower" sequence (pre-distillation tower - main distillation tower - post-treatment tower) to improve purity, requiring condensation and reflux equipment and systems. This necessitates complex equipment and cumbersome piping, leading to reduced purification efficiency. Therefore, a device that integrates distillation and impurity removal is needed to eliminate excessive and complex equipment and connecting pipelines, save space resources, and reduce maintenance difficulty. Utility Model Content

[0004] This invention addresses the technical problem of low purification efficiency caused by the complex and numerous equipment required in the carbon tetrachloride distillation and purification process. It provides an integrated carbon tetrachloride distillation and purification device, comprising a distillation column, a reflux tank, an alkaline washing and layering tank, and an azeotropic column. The distillation column has a feed inlet on its middle side, and a first outlet and a second outlet at its bottom and top, respectively. The second outlet is connected to a top condenser via a pipe. The top condenser is located directly above the reflux tank and connected to one side of the reflux tank via a pipe. One end of the reflux tank is connected to a reflux pump, and the end of the reflux pump is connected to the top of the distillation column to form a circulation pipeline.

[0005] A dual-path condenser is provided below the reflux tank. The top of the dual-path condenser is connected to a first condenser tube and a second condenser tube. The second condenser tube is connected to the other end of the reflux tank. The first condenser tube is connected to the top of the azeotropic tower through a pipe. The bottom of the dual-path condenser is provided with two condensate outlets corresponding to the first condenser tube and the second condenser tube. Both condensate outlets are connected directly to the top of the alkaline washing and layering tank through pipes. An azeotropic pipe is provided on one side of the bottom of the alkaline washing and layering tank. The end of the azeotropic pipe is connected to one side of the bottom of the azeotropic tower. The bottom and top of the azeotropic tower are respectively provided with a top outlet and a bottom outlet.

[0006] Preferably, in the above technical solution, the bottom of the distillation column is provided with a steam injection ring, and multiple injection ports are evenly distributed on the inner ring side of the steam injection ring.

[0007] Preferably, in the above technical solution, the alkaline washing stratification tank includes an alkaline washing chamber and a settling tank, with the alkaline washing chamber located above the settling tank.

[0008] Preferably, in the above technical solution, a variable frequency motor is fixedly connected to the top center of the alkali washing tank, and a stirring blade is connected to the rotation output end of the variable frequency motor.

[0009] Preferably, in the above technical solution, a connecting pipe is provided between the alkaline washing tank and the settling tank, and a second electric control valve is provided on the outer side of the top of the connecting pipe, and the settling tank is a trapezoidal column.

[0010] Preferably, in the above technical solution, a circulation pipe is connected to one side of the trapezoidal upper part of the settling tank, and the end of the circulation pipe is connected to the upper part of the alkaline washing chamber to form an internal circulation of the settling tank.

[0011] Preferably, in the above technical solution, a second centrifugal pump is connected to the bottom of the circulation pipeline.

[0012] Preferably, in the above technical solution, the pipelines between the distillation column and the top condenser, and between the reflux tank and the distillation column are all equipped with a first electric control valve, and the first condenser tube and the second condenser tube are also equipped with a first electric control valve.

[0013] Preferably, in the above technical solution, temperature sensors are provided on the inner sides of both the bottom and top of the distillation column and the azeotropic column.

[0014] Compared with the prior art, the present invention has the following beneficial effects:

[0015] This invention integrates the distillation column, reflux tank, alkali washing separator, and azeotropic tower into a single unit, eliminating the need for complex multi-device and piping connections, saving equipment space, and reducing manufacturing costs and maintenance complexity. Furthermore, by utilizing a dual-circuit condenser, different processes can be cooled simultaneously, further reducing the number of devices and the complexity of piping connections.

[0016] This invention separates the alkaline washing and settling phases by designing a layered alkaline washing tank, and uses a circulation pipeline and a second centrifugal pump to recycle the alkaline solution, thereby saving alkaline solution and improving the purification efficiency of carbon tetrachloride while filtering out chloroform.

[0017] This invention connects the top gas outlet of the azeotropic tower to the reflux port of the alkaline washing stratification tank via a condenser, allowing the azeotrope to be condensed and returned to the previous process, thus realizing internal circulation and efficient utilization of materials. Attached Figure Description

[0018] Figure 1 This is a schematic diagram of the overall structure of an integrated carbon tetrachloride distillation and impurity removal device according to the present invention;

[0019] Figure 2 This is a schematic diagram of the internal structure of the alkaline washing and stratification tank of an integrated carbon tetrachloride distillation and impurity removal device according to this utility model;

[0020] Figure 3 for Figure 1 A magnified view of the connection between the steam injection ring and the distillation column.

[0021] Explanation of key figure labels:

[0022] 1-Distillation column, 2-Top condenser, 3-Reflux tank, 4-Dual-path condenser, 5-Alkali washing stratification tank, 6-Azeotropic column, 7-First electric control valve, 8-Temperature sensor, 11-Inlet, 12-First outlet, 13-Second outlet, 14-Steam jet ring, 31-Reflux pump, 32-Reflux pipe, 41-First condenser tube, 42-Second condenser tube, 43-Condensate outlet, 51-First centrifugal pump, 52-Alkali washing chamber, 53-Variable frequency motor, 54-Stirring blade, 55-Connecting pipe, 56-Second electric control valve, 57-Settling tank, 58-Circulation pipe, 59-Second centrifugal pump, 61-Azeotropic pipe, 62-Top outlet, 63-Bottom outlet, 141-Jet nozzle. Detailed Implementation

[0023] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0024] like Figures 1-3As shown, this utility model discloses an integrated carbon tetrachloride distillation and impurity removal device, comprising a distillation column 1, a reflux tank 3, an alkaline washing and stratification tank 5, and an azeotropic column 6. The distillation column 1 has a feed inlet 11 on its middle side, and a first outlet 12 and a second outlet 13 at its bottom and top, respectively. The second outlet 13 is connected to a top condenser 2 via a pipe. The top condenser 2 is located directly above the reflux tank 3 and is connected to one side of the reflux tank 3 via a pipe. One end of the reflux tank 3 is connected to a reflux pump 31, and the end of the reflux pump 31 is connected to the top of the distillation column 1 to form a circulation pipeline. Inside the column, by controlling the pressure at the bottom of the column (0.044 MPaG), distillation is carried out using the boiling point difference between carbon tetrachloride (76.8℃) and chloroform (61.15℃). Lighter components such as chloroform, which have lower boiling points, tend to distill off from the top of the column, while heavier components with higher boiling points are enriched at the bottom of the column. Vapor rich in carbon tetrachloride and chloroform flows out from the second outlet 13, while the heavy component residue at the bottom of the column flows out from the first outlet 12 and is sent to the heavy component storage tank, and finally to the incinerator for treatment. After condensation, the liquid flows into the reflux tank 3, and most of the liquid in the reflux tank 3 is pumped back to the top of the refining column by the reflux pump to maintain a stable gas-liquid balance and distillation efficiency within the column. A dual-path condenser 4 is located below the reflux tank 3. The top of the dual-path condenser 4 is connected to a first condensing pipe 41 and a second condensing pipe 42. The second condensing pipe 42 is connected to the other end of the reflux tank 3. The first condensing pipe 41 is connected to the top of the azeotropic tower 6 via a pipe. The bottom of the dual-path condenser 4 has two condensate outlets 43 corresponding to the first condensing pipe 41 and the second condensing pipe 42. Both condensate outlets 43 are connected directly to the top of the alkaline washing layering tank 5 via pipes. An azeotropic pipe 61 is located on one side of the bottom of the alkaline washing layering tank 5. The end of the azeotropic pipe 61 is connected to one side of the bottom of the azeotropic tower 6. The azeotropic tower 6 has a top outlet 62 and a bottom outlet 63 at its bottom and top, respectively. The dual-path condenser 4 has two independent condensing pipes inside, integrating the condensation processes of different flows. This reduces the number of condensers and connecting pipes without affecting the condensation effect, thus simplifying the setup of the condensers and pipes.

[0025] It should be further explained that the pipelines between the distillation column 1 and the top condenser 2, and between the reflux tank 3 and the distillation column 1, are all equipped with first electrically controlled valves 7. The first condenser tube 41 and the second condenser tube 42 are also equipped with first electrically controlled valves 7. The first electrically controlled valves 7 can effectively control the connectivity between the various devices, further maintaining a stable gas-liquid balance and distillation efficiency within the distillation column 1. A steam injection ring 14 is provided at the bottom of the distillation column 1, and multiple injection ports 141 are evenly distributed on the inner ring side of the steam injection ring 14. The steam injection ring 14 can inject steam at different temperatures to heat the raw material to a suitable temperature and utilize the difference in boiling point temperature for preliminary impurity removal. The distillation column 1 utilizes steam to heat the raw material to improve thermal efficiency.

[0026] In this embodiment, the alkaline washing stratification tank 5 includes an alkaline washing chamber 52 and a settling tank 57, with the alkaline washing chamber 52 located above the settling tank 57. The drawn-out material, after cooling, enters the alkaline washing chamber 52 and is thoroughly mixed with a 10% alkaline solution. A variable frequency motor 53 is fixedly connected to the center of the top of the alkaline washing chamber 52, and a stirring blade 54 is connected to the rotation output end of the variable frequency motor 53. A connecting pipe 55 is provided between the alkaline washing chamber 52 and the settling tank 57, and a second electric control valve 56 is provided on the outer side of the top of the connecting pipe 55. The settling tank 57 is a trapezoidal column. By driving the rotation of the stirring blade 54 by the variable frequency motor 53, the mixing rate of the material and the alkaline solution can be effectively increased, ensuring complete reaction. A circulation pipe 58 is connected to one side of the upper trapezoidal part of the settling tank 57, and the end of the circulation pipe 58 is connected to the upper part of the alkaline washing chamber 52 to form an internal circulation within the settling tank 57. A second centrifugal pump 59 is connected to the bottom of the circulation pipe 58. After the reaction is complete, the second electric control valve 56 is opened, allowing the mixture to enter the settling tank 57 under gravity, where it naturally separates into layers due to density differences. The upper layer is a dilute alkali solution layer, and the lower layer is an organic phase mainly composed of carbon tetrachloride. At this point, some chloroform has reacted with the alkali or been dissolved and carried away, thus being removed. The carbon tetrachloride from the alkali washing process is then pumped into the azeotropic tower 6. By precisely controlling the temperature at the bottom of the tower (44°C) and the top of the tower (39.5°C), deep dehydration is performed, and the water-carbon tetrachloride azeotrope carries away any remaining trace amounts of chloroform. The azeotropic steam enters the dual-path condenser 4 from the top outlet 62 and is condensed. The condensate, containing most of the water, is returned to the alkali washing chamber 52 in the alkali washing layering tank 5 through a pipeline, forming an internal circulation. This process both recovers carbon tetrachloride and utilizes the drainage flow of the alkali washing system. The treated, high-purity carbon tetrachloride product is obtained from the bottom outlet 6.

[0027] In this embodiment, temperature control is a crucial factor determining the purity of carbon tetrachloride. Therefore, temperature sensors 8 are installed inside the reboiler and top of both distillation column 1 and azeotropic column 6. By installing temperature sensors 8 inside the reboiler and top of the column and connecting their temperature signals to the control center, operators can more intuitively observe the real-time temperatures of the reboiler and top of distillation column 1 and azeotropic column 6, thereby controlling the operating temperatures of distillation column 1 and azeotropic column 6. This control can be automated by a system preset by the control center or manually controlled by the operator.

[0028] This invention integrates a distillation column, reflux tank, alkaline washing separator, and azeotropic column into a single unit, eliminating complex multi-device and piping connections, saving equipment space, and reducing manufacturing costs and maintenance difficulty. By utilizing a dual-circuit condenser, different processes are simultaneously cooled, further reducing the number of devices and the complexity of piping connections. The alkaline washing separator is designed with separate alkaline washing and settling phases, and a circulating pipeline and a second centrifugal pump enable the recycling of the alkaline solution, saving alkaline solution and improving the purification efficiency of carbon tetrachloride while filtering out chloroform. The gas outlet at the top of the azeotropic column is connected to the reflux port of the alkaline washing separator via a condenser, allowing the condensed azeotrope to return to the preceding process, achieving internal material circulation and efficient utilization. This invention solves the technical problem of low purification efficiency caused by the complex and numerous equipment required in the carbon tetrachloride distillation and purification process. It achieves continuous material processing and targeted waste treatment, improving production efficiency and meeting environmental protection requirements.

[0029] Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. An integrated carbon tetrachloride distillation and impurity removal device, characterized in that: The distillation column (1), reflux tank (3), alkaline washing and stratification tank (5), and azeotropic column (6) are included. The distillation column (1) has a feed inlet (11) on the middle side, and a first outlet (12) and a second outlet (13) on the bottom and top, respectively. The second outlet (13) is connected to a top condenser (2) through a pipe. The top condenser (2) is located directly above the reflux tank (3) and is connected to one side of the reflux tank (3) through a pipe. One end of the reflux tank (3) is connected to a reflux pump (31), and the end of the reflux pump (31) is connected to the top of the distillation column (1) to form a circulation pipeline. A dual-path condenser (4) is provided below the reflux tank (3). The top of the dual-path condenser (4) is connected to a first condenser tube (41) and a second condenser tube (42). The second condenser tube (42) is connected to the other end of the reflux tank (3). The first condenser tube (41) is connected to the top of the azeotropic tower (6) through a pipe. The bottom of the dual-path condenser (4) is provided with two condensate outlets (43) corresponding to the first condenser tube (41) and the second condenser tube (42). Both condensate outlets (43) are connected directly to the top of the alkaline washing layer tank (5) through pipes. An azeotropic pipe (61) is provided on one side of the bottom of the alkaline washing layer tank (5). The end of the azeotropic pipe (61) is connected to one side of the bottom of the azeotropic tower (6). The bottom and top of the azeotropic tower (6) are respectively provided with a top outlet (62) and a bottom outlet (63).

2. The integrated carbon tetrachloride distillation and impurity removal device according to claim 1, characterized in that: The bottom of the distillation column (1) is provided with a steam injection ring (14), and multiple injection ports (141) are evenly distributed on the inner ring side of the steam injection ring (14).

3. The integrated carbon tetrachloride distillation and impurity removal device according to claim 1, characterized in that: The alkaline washing stratification tank (5) includes an alkaline washing chamber (52) and a settling tank (57), with the alkaline washing chamber (52) located above the settling tank (57).

4. The integrated carbon tetrachloride distillation and impurity removal device according to claim 3, characterized in that: A variable frequency motor (53) is fixedly connected to the top center of the alkaline washing chamber (52), and a stirring blade (54) is connected to the rotation output end of the variable frequency motor (53).

5. The integrated carbon tetrachloride distillation and impurity removal device according to claim 4, characterized in that: A connecting pipe (55) is provided between the alkaline washing tank (52) and the settling tank (57). A second electric control valve (56) is provided on the outer side of the top of the connecting pipe (55). The settling tank (57) is a trapezoidal column.

6. The integrated carbon tetrachloride distillation and impurity removal device according to claim 5, characterized in that: The upper trapezoidal side of the settling tank (57) is connected to a circulation pipe (58), and the end of the circulation pipe (58) is connected to the upper part of the alkaline washing chamber (52) to form an internal circulation of the settling tank (57).

7. The integrated carbon tetrachloride distillation and impurity removal device according to claim 6, characterized in that: The bottom of the circulation pipe (58) is connected to a second centrifugal pump (59).

8. The integrated carbon tetrachloride distillation and impurity removal device according to claim 1, characterized in that: The pipelines between the distillation column (1) and the top condenser (2), and between the reflux tank (3) and the distillation column (1) are all equipped with a first electric control valve (7), and the first condenser tube (41) and the second condenser tube (42) are also equipped with a first electric control valve (7).

9. The integrated carbon tetrachloride distillation and impurity removal device according to claim 1, characterized in that: Temperature sensors (8) are provided on the inner sides of the bottom and top of both the distillation column (1) and the azeotropic column (6).

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