Low-energy-consumption methane chloride production rectification system

Abstract

The utility model discloses a low-energy-consumption methane chloride production rectification system, which relates to the field of methane chloride production and comprises a crude product tank, a dichloro rectification component, a chloroform rectification component, a chloroform rectification component, a chloroform rectification component, a chloroform rectification component, a chloroform rectification component and a chloroform rectification component. The feeding adjusting valve is arranged between a discharging port of the dichloro rectification assembly and the chloroform rectification assembly, the compensation assembly is arranged between a discharging port of the dichloro rectification assembly and the chloroform rectification assembly, the liquid level control valve is arranged between the compensation assembly and a discharging port of the dichloro rectification assembly, the coarse four-carbon storage tank is connected with a discharging port of the chloroform rectification assembly, and the coarse four-carbon storage tank is connected with a discharging port of the chloroform rectification assembly. The feeding pump is arranged between the crude product tank and the dichloro rectification assembly; according to the low-energy-consumption methane chloride production rectification system, energy waste can be reduced, the stability of the rectification process is improved, and the product quality is ensured.

Description

TECHNICAL FIELD

[0001] The utility model relates to the production field of methane chloride, concretely is a low energy consumption methane chloride production rectification system. BACKGROUND

[0002] In the production process of methane chloride, the crude product obtained by reaction usually contains dichloromethane, chloroform (also known as chloroform) and carbon tetrachloride and other components. In order to effectively separate these components, dichloromethane rectification column is usually used to extract low-boiling-point dichloromethane. But directly introducing all the materials flowing out of the dichloromethane rectification column into the chloroform column will affect the stability of chloroform rectification due to the instability of dichloromethane rectification column discharge, and will cause the pressure of steam in the chloroform rectification column to change, thereby affecting the rectification effect.

[0003] Therefore, in the traditional rectification process, low-boiling-point dichloromethane is first rectified by the dichloromethane rectification column, and the materials flowing out of the dichloromethane rectification column are cooled and then enter the crude chloroform storage tank, and are then pumped and delivered to the chloroform rectification column for further rectification.

[0004] However, the materials flowing out of the dichloromethane rectification column need to be reheated when entering the chloroform rectification column, and this material processing method of cooling and then reheating will cause energy waste, and the direct entry of cold materials into the chloroform rectification column will cause the heating process to be unstable and will easily cause temperature fluctuations in the chloroform rectification process, thereby affecting product quality. UTILITY MODEL CONTENTS

[0005] The utility model aims at providing a low energy consumption methane chloride production rectification system which can reduce energy waste, improve the stability of the rectification process and ensure product quality.

[0006] The above-mentioned optimized structure of the utility model is realized by the following technical scheme: a low energy consumption methane chloride production rectification system, comprising a crude product tank, the crude product tank stores crude product;

[0007] A dichloromethane rectification assembly is connected with the crude product tank;

[0008] A chloroform rectification assembly is connected with the dichloromethane rectification assembly;

[0009] A feed regulating valve is arranged between the discharge port of the dichloromethane rectification assembly and the chloroform rectification assembly;

[0010] A compensation assembly is arranged between the discharge port of the dichloromethane rectification assembly and the chloroform rectification assembly;

[0011] a level control valve disposed between the make-up assembly and a discharge outlet of the dichloromethane distillation assembly;

[0012] a crude tetracarbon storage tank connected to a discharge outlet of the chloroform distillation assembly;

[0013] a feed pump disposed between the crude product tank and the dichloromethane distillation assembly.

[0014] In some embodiments, the make-up assembly includes a crude chloroform storage tank disposed between the level control valve and the chloroform distillation assembly;

[0015] a make-up pump disposed between the crude chloroform storage tank and the chloroform distillation assembly;

[0016] a feed make-up valve disposed between the make-up pump and the chloroform distillation assembly.

[0017] In some embodiments, further comprising a dichloromethane column bottom cooler disposed between the discharge outlet of the dichloromethane distillation assembly and the level control valve.

[0018] In some embodiments, the dichloromethane distillation assembly includes a dichloromethane distillation upper column, a feed inlet of the dichloromethane distillation upper column connected to the feed pump, a discharge outlet of the dichloromethane distillation upper column connected to the feed adjustment valve, the level control valve;

[0019] a dichloromethane reboiler connected to the dichloromethane distillation upper column;

[0020] a dichloromethane distillation lower column connected to a gas outlet of the dichloromethane distillation upper column.

[0021] In some embodiments, the dichloromethane distillation assembly further includes a dichloromethane reflux pump disposed between a discharge outlet of the dichloromethane distillation lower column and a feed inlet of the dichloromethane distillation upper column;

[0022] a dichloromethane reflux valve disposed between the dichloromethane reflux pump and the feed inlet of the dichloromethane distillation upper column.

[0023] In some embodiments, the chloroform distillation assembly includes a chloroform distillation upper column, a feed inlet of the chloroform distillation upper column connected to the feed adjustment valve, the make-up assembly;

[0024] a chloroform reboiler connected to the chloroform distillation upper column;

[0025] a chloroform distillation lower column connected to a gas outlet of the chloroform distillation upper column;

[0026] A chloroform bottom cooler is disposed between the outlet of the chloroform rectification upper column and the crude tetratomic storage tank.

[0027] In some embodiments, the chloroform rectification assembly further comprises a chloroform reflux pump disposed between the outlet of the chloroform rectification lower column and the inlet of the chloroform rectification upper column;

[0028] A chloroform reflux valve is disposed between the chloroform reflux pump and the inlet of the chloroform rectification upper column.

[0029] In summary, the present application has the following advantages:

[0030] The low-energy-consumption methane chloride production rectification system controls the stable flow of the material from the dichloro rectification assembly to the chloroform rectification assembly through the feed regulating valve, and compensates when the material outflow of the dichloro rectification assembly is insufficient, and stores the material in the compensation assembly when the material outflow of the dichloro rectification assembly is excessive, so as to realize the stable and controllable feed amount of the chloroform rectification assembly, fully utilize the heat energy of the outflow material of the dichloro rectification assembly, reduce energy waste, control the height of the liquid level in the dichloro rectification assembly through the liquid level control valve, realize the stability of the liquid level in the dichloro reboiler, avoid the influence of the liquid level fluctuation in the dichloro reboiler on the heat exchange area, and thus stabilize and improve the stability of the rectification process, and ensure the product quality. BRIEF DESCRIPTION OF DRAWINGS

[0031] Figure 1 The figure is a structural schematic diagram of the present application.

[0032] In the figure: 1, crude product tank; 2, dichloro rectification assembly; 21, dichloro rectification upper column; 22, dichloro reboiler; 23, dichloro rectification lower column; 24, dichloro reflux pump; 25, dichloro reflux valve; 3, chloroform rectification assembly; 31, chloroform rectification upper column; 32, chloroform reboiler; 33, chloroform rectification lower column; 34, chloroform bottom cooler; 35, chloroform reflux pump; 36, chloroform reflux valve; 4, feed regulating valve; 5, compensation assembly; 51, crude chloroform storage tank; 52, compensation pump; 53, feed compensation valve; 6, liquid level control valve; 7, crude tetratomic storage tank; 8, feeding pump; 9, dichloro bottom cooler. DETAILED DESCRIPTION

[0033] The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0034] Reference Figure 1 A low-energy consumption methane chloride production rectification system, comprising a crude product tank 1, a dichloro rectification assembly 2, a chloroform rectification assembly 3, a feed adjusting valve 4, a compensation assembly 5, a liquid level control valve 6, a crude four-carbon storage tank 7 and a feeding pump 8, the crude product tank 1 stores crude products, the crude products contain dichloromethane, chloroform, carbon tetrachloride and the like, the dichloro rectification assembly 2 is connected with the crude product tank 1, the feeding pump 8 is arranged between the crude product tank 1 and the dichloro rectification assembly 2, and the crude products are transported to the dichloro rectification assembly 2 for rectification to obtain chloroform products, the chloroform rectification assembly 3 is connected with the dichloro rectification assembly 2, the feed adjusting valve 4 is arranged between a discharge port of the dichloro rectification assembly 2 and the chloroform rectification assembly 3, can adjust the flow of the chloroform products entering the chloroform rectification assembly 3, the compensation assembly 5 is arranged between the discharge port of the dichloro rectification assembly 2 and the chloroform rectification assembly 3, can compensate the chloroform products entering the chloroform rectification assembly 3 to maintain the stability of the chloroform product flow, the liquid level control valve 6 is arranged between the compensation assembly 5 and the discharge port of the dichloro rectification assembly 2, can control the height of the liquid level in the dichloro rectification assembly 2 through the liquid level control valve 6, and the crude four-carbon storage tank 7 is connected with a discharge port of the chloroform rectification assembly 3 and can store the products after rectification.

[0035] Through the feed adjusting valve 4, the stable flow of the material from the dichloro rectification assembly 2 to the chloroform rectification assembly 3 is controlled (the flow is less than the required feed amount of the chloroform rectification assembly 3), through the compensation assembly 5, when the material flow of the dichloro rectification assembly 2 is insufficient, compensation is performed, when the material flow of the dichloro rectification assembly 2 is excessive, the material is stored in the compensation assembly 5, so that the feed amount of the chloroform rectification assembly 3 is stably controllable, so that the heat energy in the material flowing out of the dichloro rectification assembly 2 can be fully utilized, energy waste is reduced, and through the liquid level control valve 6, the height of the liquid level in the dichloro rectification assembly 2 is controlled, the stability of the liquid level in the dichloro reboiler 22 is realized, the fluctuation of the liquid level in the dichloro reboiler 22 is avoided, the heat exchange area is affected, so that the stability of the rectification process is improved, and the product quality is ensured.

[0036] In some embodiments, the compensation assembly 5 comprises a crude chloroform storage tank 51, a compensation pump 52 and a feed compensation valve 53, the crude chloroform storage tank 51 is arranged between the liquid level control valve 6 and the chloroform rectification assembly 3, can store the material when the material flowing out of the dichloro rectification assembly 2 is excessive, and facilitates supplementing the material when the material flowing out of the dichloro rectification assembly 2 is insufficient, so as to ensure the stable operation of the chloroform rectification assembly 3, the compensation pump 52 is arranged between the crude chloroform storage tank 51 and the chloroform rectification assembly 3, the feed compensation valve 53 is arranged between the compensation pump 52 and the chloroform rectification assembly 3, the material flow of the crude chloroform storage tank 51 to the chloroform rectification assembly 3 is controlled through the feed compensation valve 53 and the compensation pump 52, so as to realize the stability of the material flow of the chloroform rectification assembly 3.

[0037] In some embodiments, a dichloro bottom cooler 9 is further included, which is arranged between the outlet of the dichloro rectification assembly 2 and the liquid level control valve 6, and can cool the material flowing out of the dichloro rectification assembly 2, facilitating the storage of the material.

[0038] In some embodiments, the dichloro rectification assembly 2 includes a dichloro rectification upper column 21, a dichloro reboiler 22, and a dichloro rectification lower column 23. The inlet of the dichloro rectification upper column 21 is connected to the feed pump 8, for receiving and processing the crude product in the crude product tank 1. The outlet of the dichloro rectification upper column 21 is connected to the feed regulating valve 4 and the liquid level control valve 6, so that the material flow between the dichloro rectification upper column 21 and the chloroform rectification assembly 3 can be stabilized through the control of the feed regulating valve 4 and the liquid level control valve 6. The dichloro reboiler 22 is connected to the dichloro rectification upper column 21, for providing necessary heat energy to facilitate the separation of the material in the rectification process, which is a prior art and will not be described here. The dichloro rectification lower column 23 is connected to the outlet of the dichloro rectification upper column 21, for receiving and processing the gas flowing out of the dichloro rectification upper column 21, further achieving the rectification and separation of the material. The top of the dichloro rectification lower column 23 can be connected to a collection tank, a column top condenser, or other devices, for collecting and processing the gaseous product after distillation, which is a prior art and will not be described here. Through the separation of the dichloro rectification upper column 21 and the dichloro rectification lower column 23, the dichloro rectification effect can be achieved while reducing the manufacturing cost of the rectification column.

[0039] In some embodiments, the dichloro rectification assembly 2 further includes a dichloro reflux pump 24 and a dichloro reflux valve 25. The dichloro reflux pump 24 is arranged between the outlet of the dichloro rectification lower column 23 and the inlet of the dichloro rectification upper column 21, for refluxing part of the processed material to the upper column to achieve more efficient rectification and separation. The dichloro reflux valve 25 is arranged between the dichloro reflux pump 24 and the inlet of the dichloro rectification upper column 21, for accurately controlling the flow of the refluxed material, ensuring the stability and efficiency of the rectification process.

[0040] In some embodiments, the chloroform rectification assembly 3 includes a chloroform rectification upper tower 31, a chloroform reboiler 32, a chloroform rectification lower tower 33, and a chloroform tower bottom cooler 34. The feed inlet of the chloroform rectification upper tower 31 is connected with the feed adjusting valve 4 and the compensation assembly 5. The chloroform reboiler 32 is connected with the chloroform rectification upper tower 31, which can provide necessary heat energy for the rectification process and promote the effective separation of the material in the tower. The chloroform rectification lower tower 33 is connected with the gas outlet of the chloroform rectification upper tower 31, which can receive and process the gas flowing out of the chloroform rectification upper tower 31, further realizing the rectification and separation of chloroform. The top of the chloroform rectification lower tower 33 can be connected with a collection tank, an overhead condenser and other devices to realize the collection and subsequent processing of the gaseous product after distillation. This is the prior art and will not be described here. The chloroform tower bottom cooler 34 is arranged between the discharge outlet of the chloroform rectification upper tower 31 and the crude four-carbon storage tank 7, which can cool the material flowing out of the chloroform rectification upper tower 31 and store the cooled material in the crude four-carbon storage tank 7 for subsequent use.

[0041] In some embodiments, the chloroform rectification assembly 3 further includes a chloroform reflux pump 35 and a chloroform reflux valve 36. The chloroform reflux pump 35 is arranged between the discharge outlet of the chloroform rectification lower tower 33 and the feed inlet of the chloroform rectification upper tower 31, which can return part of the processed material to the chloroform rectification upper tower 31 to improve the efficiency and purity of the rectification and separation. The chloroform reflux valve 36 is arranged between the chloroform reflux pump 35 and the feed inlet of the chloroform rectification upper tower 31, which can accurately control the flow of the reflux material to ensure the stability and efficiency of the rectification process, thereby obtaining chloroform products with higher quality.

[0042] In some embodiments, a control system is further included, which is electrically connected with the dichloromethane rectification assembly 2, the chloroform rectification assembly 3, the feed adjusting valve 4, the compensation assembly 5, the liquid level control valve 6 and the feeding pump 8. The feed adjusting valve 4, the compensation assembly 5 and the liquid level control valve 6 can be solenoid control valves, which have the advantages of fast response and high efficiency control and can be wirelessly connected. The feed adjusting valve 4, the compensation assembly 5 and the liquid level control valve 6 feed back values to the control system, which adjusts the working state of the feed adjusting valve 4, the compensation assembly 5 and the liquid level control valve 6, such as opening, closing, opening and closing degree, etc., to realize stable feeding of the chloroform rectification assembly 3. At the same time, the steam flow of the chloroform reboiler 32 can be controlled according to the flow of the material, so that the steam in the chloroform rectification assembly 3 is adjusted in time with the feeding temperature to ensure that the rectification tower product is qualified. In this process, the flow of the feed adjusting valve 4 is as stable as possible and accounts for a large proportion, so that the variable flow of the compensation assembly 5 accounts for a small proportion, and thus the temperature fluctuation of the material entering the chloroform rectification assembly 3 is small.

[0043] The specific working principle is as follows:

[0044] The crude product obtained in the reaction in the production of methane chloride is stored in a crude product tank 1 and is delivered by a feeding pump 8 to a dichloromethane rectification assembly 2 for rectification. The dichloromethane rectification assembly 2 rectifies low-boiling dichloromethane out, and the rectified material is partly introduced into a chloroform rectification assembly 3 under the control of a feed regulating valve 4, and the other part is cooled by a dichloromethane bottom cooler 9 and then stored in a crude chloroform storage tank 51.

[0045] When the flow of the rectified material of the dichloromethane rectification assembly 2 cannot meet the feed requirement of the chloroform rectification assembly 3, a feed compensation valve 53 is opened, and a compensation pump 52 delivers the material in the crude chloroform storage tank 51 to the chloroform rectification assembly 3 under pressure, the chloroform rectification assembly 3 rectifies chloroform out, and the rectified product in the chloroform rectification assembly 3 is cooled by a chloroform bottom cooler 34 and then stored in a crude four-carbon storage tank 7.

[0046] The above examples are only used to illustrate the technical solutions of the present application, but not to limit it; although the present application has been described in detail with reference to the foregoing examples, those skilled in the art should understand that the technical solutions recorded in the foregoing examples can still be modified, or some technical features can be replaced equivalently; and these modifications or replacements do not make the essence of the corresponding technical solutions deviate from the spirit and scope of the technical solutions of the embodiments of the present application.

Claims

1. A low energy consumption methane chloride production rectification system characterized by: The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8).

2. A low energy consumption production of methane chlorides distillation system according to claim 1, characterized in that: The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8).

3. A low energy consumption process for the production of methane chlorides by rectification according to claim 1, characterized in that: The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8).

4. A low energy consumption process for the production of methane chlorides by rectification according to claim 1, characterized in that: The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8).

5. A low energy consumption process for the production of methane chlorides by rectification according to claim 4, characterized in that: The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8).

6. A low energy consumption process for the production of methane chlorides according to claim 1, characterized in that: The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with the crude four-carbon storage tank (7), and the crude product tank (1) is connected with the feeding pump (8). The crude product tank (1) is connected with the dichloro distillation assembly (2), the dichloro distillation assembly (2) is connected with the chloroform distillation assembly (3), the chloroform distillation assembly (3) is connected with A chloroform bottom cooler (34) is arranged between the discharge port of the chloroform rectification upper column (31) and the crude four-carbon storage tank (7).

7. A low energy consumption process for the production of methane chlorides by rectification according to claim 6, characterized in that: The chloroform rectification assembly (3) further comprises a chloroform reflux pump (35) arranged between the discharge port of the chloroform rectification lower column (33) and the feed port of the chloroform rectification upper column (31); A chloroform reflux valve (36) is arranged between the chloroform reflux pump (35) and the feed port of the chloroform rectification upper column (31).

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