Ethylcarbazole high-efficiency rectification purification system
By designing a high-efficiency distillation purification system that includes an atmospheric pressure tower, a primary distillation packed tower, and a rectification packed tower, the problems of limited purity improvement and high energy consumption in the purification process of ethylcarbazole were solved. This system achieves efficient recovery of high-purity ethylcarbazole and toluene-like organic compounds, reduces energy consumption, and increases equipment throughput.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- GREENSEA HYDROGEN ENERGY TECHNOLOGY (SUZHOU) CO LTD
- Filing Date
- 2025-06-25
- Publication Date
- 2026-07-14
AI Technical Summary
Existing technologies for the purification of ethylcarbazole suffer from problems such as severe pollution from solvent methods, low efficiency of static crystallization methods, and low separation efficiency of distillation methods. Furthermore, they are difficult to effectively separate ethylcarbazole from impurities, resulting in limited improvement in purity.
A high-efficiency distillation purification system comprising an atmospheric distillation column, a primary distillation packed column, and a rectification packed column is adopted. Through the combination of a circulating pump, a reboiler, a heat exchanger, and a reflux ratio adjustment mechanism, continuous operation and efficient separation are achieved, reducing energy consumption and improving recovery rate.
The purity of ethylcarbazole reaches 99.2%-99.5%, the recovery rate of toluene-like organic matter is increased by 90%, energy consumption is reduced by 30%, there is no wastewater discharge, the equipment has a processing capacity of 1 ton/day, and it has high industrial feasibility.
Smart Images
Figure CN224484980U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the technical field of distillation and separation systems, and in particular to a high-efficiency distillation and purification system for ethylcarbazole. Background Technology
[0002] Ethylcarbazole is an important organic hydrogen storage material and dye intermediate, and its purity directly affects its performance in downstream applications. Traditional purification methods include solvent crystallization (such as ethanol washing), static distribution crystallization, and azeotropic distillation, but these methods have the following problems:
[0003] 1. Solvent method: Requires the use of large amounts of ethanol or DMF, generating wastewater pollution, and the product purity is difficult to exceed 95%;
[0004] 2. Static crystallization method: Intermittent operation is inefficient, easily forms powdery crystals leading to high moisture content, and has limited effect on improving purity;
[0005] 3. Distillation method: Ethyl carbazole and impurities (such as carbazole, phenanthrene, anthracene) have similar boiling points (ethyl carbazole boiling point is about 340-345℃, carbazole 355℃, phenanthrene 337℃). Conventional distillation separation efficiency is low, and high temperature can easily cause the material to coke.
[0006] Chinese patent CN112250613A discloses a device system for continuous cooling recrystallization of ethylcarbazole, which uses continuous cooling crystallization combined with ultrasonic crushing, but requires multiple crystallization steps and the equipment is complex.
[0007] Chinese patent CN206473847U discloses a differential pressure distillation system, including a first atmospheric pressure distillation packed column, a pressurized distillation packed column, and a second atmospheric pressure distillation packed column. The top outlet of the first atmospheric pressure distillation packed column is connected to the inlet of the pressurized distillation packed column, and the top outlet of the pressurized distillation packed column is connected to the inlet of the second atmospheric pressure distillation packed column. In this system, the lighter components produced by the previous distillation column are further separated each time, and high-purity methyl ethyl ketone (MEK) is finally separated from the methanol-MEK-water system. Here, the boiling point order is water > methanol > MEK, so MEK is the lightest phase and can be separated using the above system. However, the impurities present in the reaction solution of ethyl carbazole are haloalkanes, benzene-based organic mixtures, and carbazole, among which ethyl carbazole is a heavier phase and is not suitable for separation using the above system.
[0008] Therefore, it is necessary to improve the system architecture to solve the above problems. Utility Model Content
[0009] The main objective of this invention is to provide a high-efficiency distillation and purification system for ethylcarbazole, which can recover ethylcarbazole and toluene-like organic compounds with high purity and has high industrial feasibility.
[0010] This utility model achieves the above objectives through the following technical solution: an ethylcarbazole high-efficiency distillation and purification system, comprising an atmospheric pressure column, a primary distillation packed column, and a rectification packed column;
[0011] The atmospheric distillation column is provided with a first bottom reflux pipe at the bottom and a first top reflux pipe at the top. A first circulating pump and a first reboiler are arranged sequentially on the first bottom reflux pipe in the direction of liquid flow. A first heat exchanger and a first reflux ratio adjustment mechanism are arranged sequentially on the first top reflux pipe in the direction of flow. One outlet of the first reflux ratio adjustment mechanism is connected to the upper part of the atmospheric distillation column, and the other outlet is connected to the first drain pipe. A second inlet pipe is provided at the middle node between the first circulating pump and the first reboiler, which connects to the middle of the primary distillation packed column. A second inlet valve is provided on the second inlet pipe.
[0012] The lower part of the primary distillation packed column is provided with a second bottom reflux pipe, and the upper part is provided with a second top reflux pipe. The second bottom reflux pipe is provided with a second circulation pump and a second reboiler in sequence according to the liquid flow direction. The second top reflux pipe is provided with a second heat exchanger and a second reflux ratio adjustment mechanism in sequence according to the flow direction. One outlet of the second reflux ratio adjustment mechanism is connected to the upper part of the primary distillation packed column, and the other outlet is connected to a second drain pipe. A third inlet pipe is provided at the middle node between the second circulation pump and the second reboiler, which is connected to the middle part of the rectification packed column. A third inlet valve is provided on the third inlet pipe.
[0013] The distillation packed column is provided with a third bottom reflux pipe at the bottom and a third top reflux pipe at the top. The third bottom reflux pipe is provided with a third circulating pump and a third reboiler in sequence according to the liquid flow direction. The third top reflux pipe is provided with a third heat exchanger and a third reflux ratio adjustment mechanism in sequence according to the flow direction. One outlet of the third reflux ratio adjustment mechanism is connected to the upper part of the distillation packed column, and the other outlet is connected to the third drain pipe.
[0014] Specifically, the middle part of the atmospheric pressure tower is connected to a first inlet pipe, and a first inlet valve is provided on the first inlet pipe.
[0015] Furthermore, filters are provided on the first inlet pipe, the second inlet pipe, the third inlet pipe, the first bottom reflux pipe, the second bottom reflux pipe, the third bottom reflux pipe, the first top reflux pipe, the second top reflux pipe, and the third top reflux pipe.
[0016] Specifically, a waste discharge pipe is provided at the middle node between the third circulating pump and the third reboiler, and a waste discharge valve is provided on the waste discharge pipe.
[0017] Specifically, the second heat exchanger is connected to the vacuum mechanism via the first suction pipe, and the third heat exchanger is connected to the vacuum mechanism via the second suction pipe.
[0018] Specifically, the outlet of the first drain pipe is connected to the first buffer tank, the outlet of the second drain pipe is connected to the second buffer tank, and the outlet of the third drain pipe is connected to the third buffer tank.
[0019] The beneficial effects of this utility model's technical solution are:
[0020] After being processed by the above distillation and purification system, the purity of ethylcarbazole can reach 99.2%-99.5%; the recovery rate of toluene-like organic matter is increased by 90%, and energy consumption is reduced by 30%; there is no wastewater discharge; continuous operation, and the processing capacity of a single set of equipment reaches 1 ton / day, making it highly feasible for industrialization. Attached Figure Description
[0021] Figure 1 This is a simplified pipeline diagram of the ethylcarbazole high-efficiency distillation purification system for an example.
[0022] The numbers in the diagram represent:
[0023] 1a - Atmospheric pressure column, 1b - Preliminary distillation packed column, 1c - Rectification packed column;
[0024] 2a-First inlet pipe, 21a-First inlet valve, 2b-Second inlet pipe, 21b-Second inlet valve, 2c-Third inlet pipe, 21c-Third inlet valve, 2d-Waste drain pipe, 21d-Waste drain valve;
[0025] 3a - First column bottom reflux pipe, 31a - First circulation pump, 32a - First reboiler, 3b - Second column bottom reflux pipe, 31b - Second circulation pump, 32b - Second reboiler, 3c - Third column bottom reflux pipe, 31c - Third circulation pump, 32c - Third reboiler;
[0026] 4a - First column top reflux pipe, 41a - First heat exchanger, 42a - First reflux ratio adjustment mechanism, 4b - Second column top reflux pipe, 41b - Second heat exchanger, 42b - Second reflux ratio adjustment mechanism, 43b - First suction pipe, 4c - Third column top reflux pipe, 41c - Third heat exchanger, 42c - Third reflux ratio adjustment mechanism, 43c - Second suction pipe;
[0027] 5a - First drain pipe, 5b - Second drain pipe, 5c - Third drain pipe;
[0028] 6a - First buffer tank, 6b - Second buffer tank, 6c - Third buffer tank;
[0029] 7-Filter. Detailed Implementation
[0030] The present invention will be further described in detail below with reference to specific embodiments.
[0031] Example:
[0032] like Figure 1 As shown, the present invention provides a high-efficiency distillation and purification system for ethyl carbazole, comprising an atmospheric pressure column 1a, a primary distillation packed column 1b, and a rectification packed column 1c.
[0033] The middle part of the atmospheric pressure tower 1a is connected to the first liquid inlet pipe 2a, and the first liquid inlet pipe 2a is equipped with a first liquid inlet valve 21a.
[0034] like Figure 1 As shown, the first inlet pipe 2a is the raw material input port of the entire distillation and purification system, used to transport the solution to be treated before purification (crude ethylcarbazole solution with a purity of 30%-50%). The first inlet valve 21a is used to control whether the solution to be treated is input.
[0035] like Figure 1 As shown, the atmospheric distillation column 1a has a first bottom reflux pipe 3a at its lower part and a first top reflux pipe 4a at its upper part. A first circulating pump 31a and a first reboiler 32a are sequentially arranged on the first bottom reflux pipe 3a according to the liquid flow direction. A second inlet pipe 2b, connecting to the middle part of the primary distillation packed column 1b, is located at the midpoint between the first circulating pump 31a and the first reboiler 32a. A second inlet valve 21b is installed on the second inlet pipe 2a. A first heat exchanger 41a and a first reflux ratio adjusting mechanism 42a are sequentially arranged on the first top reflux pipe 4a according to the flow direction. One outlet of the first reflux ratio adjusting mechanism 42a is connected to the upper part of the atmospheric distillation column 1a, and the other outlet is connected to a first drain pipe 5a. The outlet of the first drain pipe 5a is connected to a first buffer tank 6a.
[0036] The first reboiler 32a and the first heat exchanger 41a jointly control the temperature within the atmospheric column 1a. The first circulating pump 31a controls the external circulation of the heavy components at the bottom of the atmospheric column 1a (when the second inlet valve 21b is closed), then replenishes heat through the first reboiler 32a, increasing the heat within this local system of the atmospheric column 1a. The first heat exchanger 41a cools and condenses the light components distilled from the top of the column. The first reflux ratio regulating mechanism 42a allows a portion of the light components to reflux back to the upper part of the atmospheric column 1a according to a set ratio, reducing the heat within this local system. Another portion of the light components is discharged through the first drain pipe 5a. The first buffer tank 6a can temporarily collect the light components distilled in the first runoff, which can be discharged together when a certain amount is reached.
[0037] like Figure 1As shown, the lower part of the primary distillation packed column 1b is equipped with a second bottom reflux pipe 3b, and the upper part is equipped with a second top reflux pipe 4b. A second circulation pump 31b and a second reboiler 32b are sequentially arranged on the second bottom reflux pipe 3b according to the liquid flow direction. A third inlet pipe 2c, connecting to the middle part of the primary distillation packed column 1b, is located at the midpoint between the second circulation pump 31b and the second reboiler 32b. A third inlet valve 21c is installed on the third inlet pipe 2c. A second heat exchanger 41b and a second reflux ratio adjusting mechanism 42b are sequentially arranged on the second top reflux pipe 4b according to the flow direction. One outlet of the second reflux ratio adjusting mechanism 42b is connected to the upper part of the primary distillation packed column 1b, and the other outlet is connected to a second drain pipe 5b. The outlet of the second drain pipe 5b is connected to a second buffer tank 6b. The second heat exchanger 41b is connected to a vacuum mechanism through a first suction pipe 43b.
[0038] The temperature control principle of the primary distillation packed column 1b is the same as that of the atmospheric distillation column 1a. The second reboiler 32b and the second heat exchanger 41b jointly control the temperature within the primary distillation packed column 1b, which will not be elaborated further. The difference lies in that the primary distillation packed column 1b can reduce the pressure within the column through the first suction pipe 43b, thereby reducing the heat required for primary distillation. The second column top reflux pipe 4b allows a portion of the light components to flow back to the upper part of the primary distillation packed column 1b according to a set ratio, while another portion of the light components is discharged through the second drain pipe 5b. The second buffer tank 6b can temporarily collect the light components from the second distillation, which can be discharged together when a certain amount is reached.
[0039] like Figure 1 As shown, the lower part of the distillation packed column 1c is equipped with a third bottom reflux pipe 3c, and the upper part is equipped with a third top reflux pipe 4c. A third circulation pump 31c and a third reboiler 32c are sequentially arranged on the third bottom reflux pipe 3c in the direction of liquid flow. A waste discharge pipe 2d is located at the midpoint between the third circulation pump 31c and the third reboiler 32c, and a waste discharge valve 21d is installed on the waste discharge pipe 2d. A third heat exchanger 41c and a third reflux ratio adjusting mechanism 42c are sequentially arranged on the third top reflux pipe 4c in the direction of flow. One outlet of the third reflux ratio adjusting mechanism 42c is connected to the upper part of the distillation packed column 1c, and the other outlet is connected to a third drain pipe 5c. The outlet of the third drain pipe 5c is connected to a third buffer tank 6c. The third heat exchanger 41c is connected to a vacuum mechanism through a second suction pipe 43c.
[0040] The temperature and pressure control principles of the distillation packed column 1c are the same as those of the primary distillation packed column 1b. Reduced pressure distillation also helps reduce energy consumption. The third column top reflux pipe 4c allows a portion of the light components to flow back to the top of the distillation packed column 1c according to a set ratio, while another portion of the light components is discharged through the second drain pipe 5b. The second buffer tank 6b can temporarily collect the light components from the second distillation, which can be discharged together when a certain amount is reached. The undistilled portion in the distillation packed column 1c is discharged through the waste discharge pipe 2d.
[0041] To reduce the risk of precipitated substances clogging the pipelines, filters 7 are installed on the first inlet pipe 2a, the second inlet pipe 2b, the third inlet pipe 2c, the first bottom reflux pipe 3a, the second bottom reflux pipe 3b, the third bottom reflux pipe 3c, the first top reflux pipe 4a, the second top reflux pipe 4b, and the third top reflux pipe 4c.
[0042] In practical applications, the pressure inside the atmospheric distillation column 1a is one atmosphere, and the temperature of the first reboiler 32a is controlled at 100~120℃. The atmospheric distillation column 1a is mainly used to remove the halogenated hydrocarbons with the lowest boiling point (the components collected in the first buffer tank 6a) from the processing liquid, while the remaining components are sent to the primary distillation packed column 1b through the second inlet pipe 2b for further separation.
[0043] The pressure inside the primary distillation packed column 1b is -0.08 to -0.1 MPa, and the temperature of the second reboiler 32b is controlled at 100 to 120℃ (the same as that of the atmospheric distillation column 1a). The primary distillation packed column 1b is mainly used to remove toluene-like organic compounds with lower boiling points (the components collected in the second buffer tank 6b) from the processing liquid, while the remaining components are sent to the rectification packed column 1c through the third inlet pipe 2c for further separation.
[0044] The pressure inside the distillation packed column 1c is -0.08 to -0.1 MPa (the same as that in the primary distillation packed column 1b), and the temperature of the third reboiler 32c is controlled at 140 to 200℃. The distillation packed column 1c is mainly used to distill off ethylcarbazole (the component collected in the third buffer tank 6c), and the residual liquid in the column contains high-boiling-point components, including carbazole derivatives.
[0045] Atmospheric pressure column 1a performs coarse separation and maintains the bottom solution temperature similar to that of primary distillation packing column 1b and rectification packing column 1c, reducing energy consumption and equipment investment, and achieving efficient recovery of haloalkanes; primary distillation packing column 1b removes low-boiling-point solvents and achieves efficient recovery of toluene-like organic compounds; rectification packing column 1c achieves efficient separation of ethylcarbazole and carbazole under reduced pressure, reducing thermosensitive decomposition.
[0046] After being processed by the above distillation and purification system, the purity of ethylcarbazole can reach 99.2%-99.5%; the recovery rate of toluene-like organic matter is increased by 90%, and energy consumption is reduced by 30%; there is no wastewater discharge; continuous operation, and the processing capacity of a single set of equipment reaches 1 ton / day, making it highly feasible for industrialization.
[0047] The above descriptions are merely some embodiments of this utility model. For those skilled in the art, various modifications and improvements can be made without departing from the inventive concept of this utility model, and all such modifications and improvements fall within the protection scope of this utility model.
Claims
1. A high-efficiency distillation purification system for ethylcarbazole, characterized in that: This includes atmospheric distillation columns, primary distillation columns, and rectification distillation columns; The atmospheric distillation column is provided with a first bottom reflux pipe at the bottom and a first top reflux pipe at the top. A first circulating pump and a first reboiler are arranged sequentially on the first bottom reflux pipe in the direction of liquid flow. A first heat exchanger and a first reflux ratio adjustment mechanism are arranged sequentially on the first top reflux pipe in the direction of flow. One outlet of the first reflux ratio adjustment mechanism is connected to the upper part of the atmospheric distillation column, and the other outlet is connected to the first drain pipe. A second inlet pipe is provided at the middle node between the first circulating pump and the first reboiler, which connects to the middle of the primary distillation packed column. A second inlet valve is provided on the second inlet pipe. The lower part of the primary distillation packed column is provided with a second bottom reflux pipe, and the upper part is provided with a second top reflux pipe. The second bottom reflux pipe is provided with a second circulation pump and a second reboiler in sequence according to the liquid flow direction. The second top reflux pipe is provided with a second heat exchanger and a second reflux ratio adjustment mechanism in sequence according to the flow direction. One outlet of the second reflux ratio adjustment mechanism is connected to the upper part of the primary distillation packed column, and the other outlet is connected to a second drain pipe. A third inlet pipe is provided at the middle node between the second circulation pump and the second reboiler, which is connected to the middle part of the rectification packed column. A third inlet valve is provided on the third inlet pipe. The distillation packed column is provided with a third bottom reflux pipe at the bottom and a third top reflux pipe at the top. The third bottom reflux pipe is provided with a third circulating pump and a third reboiler in sequence according to the liquid flow direction. The third top reflux pipe is provided with a third heat exchanger and a third reflux ratio adjustment mechanism in sequence according to the flow direction. One outlet of the third reflux ratio adjustment mechanism is connected to the upper part of the distillation packed column, and the other outlet is connected to the third drain pipe.
2. The high-efficiency distillation and purification system for ethylcarbazole according to claim 1, characterized in that: The atmospheric pressure tower is connected to a first inlet pipe in the middle, and a first inlet valve is provided on the first inlet pipe.
3. The high-efficiency distillation and purification system for ethylcarbazole according to claim 2, characterized in that: The first inlet pipe, the second inlet pipe, the third inlet pipe, the first bottom reflux pipe, the second bottom reflux pipe, the third bottom reflux pipe, the first top reflux pipe, the second top reflux pipe, and the third top reflux pipe are all equipped with filters.
4. The high-efficiency distillation and purification system for ethylcarbazole according to claim 1, characterized in that: A waste discharge pipe is provided at the middle node between the third circulating pump and the third reboiler, and a waste discharge valve is provided on the waste discharge pipe.
5. The high-efficiency distillation and purification system for ethylcarbazole according to claim 1, characterized in that: The second heat exchanger is connected to the vacuum mechanism via the first suction pipe, and the third heat exchanger is connected to the vacuum mechanism via the second suction pipe.
6. The high-efficiency distillation and purification system for ethylcarbazole according to claim 1, characterized in that: The outlet of the first drain pipe is connected to the first buffer tank, the outlet of the second drain pipe is connected to the second buffer tank, and the outlet of the third drain pipe is connected to the third buffer tank.