Chloride purification system and method

By designing a chloride purification system, the combination of a still kettle, reflux assembly and receiving tube is used to achieve efficient purification of chloride, solving the problem of insufficient purity of chloride in China, improving product quality and autonomy, and reducing production costs .

CN119280864AInactive Publication Date: 2025-01-10广东长信精密设备有限公司
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Patent Information

Application Number
CN202411829911.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-12
Publication Date
2025-01-10
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

my country's existing chloride production technology is difficult to meet the strict requirements of the chemical vapor precipitation process on the purity of chloride, resulting in a decline in the quality and unstable performance of the deposited film, and its dependence on foreign imports increases production costs and risks.

Method used

A chloride purification system including a still kettle, a reflux assembly and a receiving tube was designed to achieve circulating reflux and condensation of steam by injecting nitrogen gas and controlling the state of the plug, collecting the pre-fraction and high-purity chlorine compounds to achieve 4.5N purity.

Benefits of technology

It effectively improves the purity of chloride, meets the requirements of chemical vapor precipitation process, reduces the difficulty of equipment use and maintenance costs, reduces the dependence on foreign imports, and enhances autonomy and competitiveness.

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Abstract

The invention relates to the technical field of separation and purification, and particularly discloses a chloride purification system which comprises a rectifying still, a backflow assembly and a receiving pipe, and the top of the rectifying still is provided with a feeding pipe, a gas injection pipe, a rectifying gas outlet pipe and a groove used for containing a thermometer; in the backflow assembly, a first pipeline is connected with a rectification gas outlet pipe, a second pipeline and a third pipeline are connected with the first pipeline and a fourth pipeline to form a quadrilateral loop, a liquid collecting pipe is connected to the joint of the second pipeline and the fourth pipeline to form a three-way branch, and a cock is arranged to control opening and closing of the liquid collecting pipe so as to switch fractionation and backflow operations; packing pieces are arranged in the first pipeline and the fourth pipeline, and the pipeline branches are controlled to be opened and closed through vertical movement of the condensation pieces and the packing pieces; a liquid inlet pipe and an exhaust pipe are arranged at the top of the receiving pipe, and the liquid inlet pipe is connected with the liquid collecting pipe. According to the chloride purification system provided by the invention, the product purity is improved, the requirements of a chemical vapor deposition process can be met, and compared with the prior art, the system is simple in structure and easy to operate and maintain.
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Description

Technical Field

[0001] The present application relates to the field of separation and purification, and in particular to a system and method for purifying chlorides. Background Art

[0002] As an important material preparation technology, chemical vapor deposition is widely used in many fields such as semiconductors and optical films. In this process, chlorine compounds are one of the key raw materials. However, since the chemical vapor deposition process has extremely strict requirements on the purity of chlorine compounds, my country's existing chlorine compound production technology is difficult to meet this standard.

[0003] Domestically produced chlorides often contain a variety of impurities, which can have a serious negative impact on the effect of the chemical vapor deposition process, such as causing the quality of the deposited film to decline, unstable performance, and even failure to meet specific application requirements. Therefore, the chlorine compounds currently used in the chemical vapor deposition process in my country mainly rely on foreign imports. This dependence not only increases production costs, but may also be restricted by various factors such as the international trade situation and supply chain stability. In today's global economic integration, trade frictions, epidemics and other emergencies may affect the import of chlorine compounds, thereby hindering the development of related industries in my country.

[0004] In order to change the current situation, enhance my country's autonomy and competitiveness in the field of chemical vapor deposition technology, achieve effective purification of existing chlorine compounds, ensure that their purity meets the requirements of chemical vapor deposition technology, and thus reduce dependence on foreign imports and promote the healthy development of related industries in my country, the research and development of a simple and economical chlorine compound purification system is imminent. Summary of the invention

[0005] In view of this, the purpose of the present application is to provide a chloride purification system to solve the problems of complex system and poor purification effect existing in the chloride purification system.

[0006] In order to achieve the above technical purpose, the present application provides a chloride purification system, including a distillation kettle 1, a reflux component 2, and a receiving tube 3.

[0007] The top of the distillation kettle 1 is provided with a feed pipe 11 connected to the outside, a gas injection pipe 12, a distillation gas outlet pipe 13, and a groove 14 formed by the top inwardly concave, which is used to place a thermometer to detect the temperature inside the distillation kettle 1; the feed pipe 11 is also provided with a grinding plug for sealing the feed pipe 11;

[0008] The reflux assembly 2 includes a first pipeline 21 connected to the rectification gas outlet pipe 13, and also includes a second pipeline 22, a third pipeline 23, a fourth pipeline 24, and a liquid collecting pipe 25; the second pipeline 22 and the third pipeline 23 are both connected end to end to the pipe walls of the first pipeline 21 and the fourth pipeline 24 to form a quadrilateral loop; one end of the liquid collecting pipe 25 is connected to the connection between the second pipeline 22 and the fourth pipeline 24 to form a three-way branch; the liquid collecting pipe 25 is also provided with a cock 26 for controlling the opening and closing state of the liquid collecting pipe 25 to switch the distillation and reflux operations;

[0009] The reflux assembly 2 further includes a condensation member 27 disposed inside the first pipe 21 and a filler member 28 disposed inside the fourth pipe 24, and the opening or closing state of the pipe wall branches of the first pipe 21 and the fourth pipe 24 is controlled by the up and down movement of the condensation member 27 and the filler member 28;

[0010] The reflux assembly 2 is also provided with a condensing device 29, which is used to condense the steam entering the first pipe 21, the second pipe 22, the third pipe 23, the fourth pipe 24, and the liquid collecting pipe 25;

[0011] The receiving tube 3 is a container with an opening on one side, and the opening of the receiving tube 3 is sealed by an end cover 33; a liquid inlet pipe 31 and an exhaust pipe 32 connected to the outside are also provided on the top of the receiving tube 3, and the liquid inlet pipe 31 is connected to the liquid collecting pipe 25 of the reflux component 2.

[0012] Furthermore, a quartz receiving boat is provided in the receiving tube 3 for receiving the distillate; the end of the liquid inlet tube 31 extends downward to the inside of the receiving tube 3 so that the distillate can flow downward along the liquid inlet tube 31 into the quartz receiving boat.

[0013] Furthermore, the lower ends of the condensation piece 27 and the filler piece 28 are provided with barbs, and the upper ends of the first pipe 21 and the fourth pipe 24 protrude into the interior of the pipe to form protruding ends, and the barbs and the protruding ends cooperate with each other to prevent the condensation piece 27 and the filler piece 28 from being sprayed off from the upper ends of the first pipe 21 and the fourth pipe 24 during the operation of the device.

[0014] Furthermore, a funnel is provided at the end of the feed pipe 11 at the top of the distillation kettle 1, so that the raw materials can smoothly enter the feed pipe 11 through the funnel.

[0015] Furthermore, it also includes an absorption tank 5 for containing absorption liquid, and the absorption tank 5 is provided with a first air inlet pipe 51 and a first air outlet pipe 52 ; the first air inlet pipe 51 is connected to the exhaust pipe 32 of the receiving pipe 3 .

[0016] Furthermore, it also includes a buffer tank 4, which is arranged between the receiving pipe 3 and the absorption tank 5; a second air inlet pipe 41 and a second air outlet pipe 42 are provided on the top of the buffer tank 4; the second air inlet pipe 41 is connected to the exhaust pipe 32 of the receiving pipe 3; the second air outlet pipe 42 is connected to the first air inlet pipe 51 of the absorption tank 5.

[0017] Further, the second air outlet pipe 42 and / or the first air inlet pipe 51 is provided with a cavity.

[0018] Furthermore, at least three cavities are provided.

[0019] Furthermore, a buffer pipe 6 is provided, the two ends of which are connected to the fourth pipe 24 and the second air intake pipe 41 .

[0020] Secondly, the present application also provides a method for purifying chloride, which is purified using a chloride purification system, and the specific steps are as follows:

[0021] Step S1, injecting nitrogen into the distillation kettle 1 through the gas injection pipe 12 to empty the distillation kettle 1, and then feeding the crude chloride into the distillation kettle 1 from the feed pipe 11, and covering the grinding plug tightly.

[0022] Step S2, control the stopcock 26 to keep the liquid collecting pipe 25 in a closed state, heat the distillation kettle 1 to 500° C., vaporize the crude chloride and enter the quadrilateral loop from the first pipeline 21 to circulate and reflux for the first period of time;

[0023] Step S3, after the reflux is completed, the stopcock 26 is opened, and the vaporized chloride is first condensed through the liquid collecting pipe 25, and then collected by the quartz boat in the receiving pipe 3 through the liquid inlet pipe 31. This is the collection process of the front fraction; wherein, the collection of the front fraction must meet the following conditions: the collection time is 1.5h or the mass of the collected front fraction accounts for 20% of the mass of the feed;

[0024] Step S4, after the collection of the current fraction is completed, the distillation kettle 1 is heated to raise the temperature by 10° C. The fraction collected at this temperature is a high-purity chlorine compound.

[0025] In summary, the chloride purification system of the present application scheme includes a distillation kettle 1, a reflux assembly 2 and a receiving pipe 3. The top of the distillation kettle 1 has a feed pipe 11, an air injection pipe 12, a distillation outlet pipe 13 and a groove 14 for placing a thermometer. In the reflux assembly 2, the first pipeline 21 is connected to the distillation outlet pipe 13, the second pipeline 22, the third pipeline 23 connects the first pipeline 21 and the fourth pipeline 24 to form a quadrilateral loop, and the collecting pipe 25 is connected to the second and fourth pipelines to form a three-way branch, and a cock 26 is provided to control the opening and closing to switch the fractionation and reflux operations. There is a condensing part 27 in the first pipeline 21, and a packing part 28 in the fourth pipeline 24, which can be moved up and down to control the opening and closing of the branch. The receiving pipe 3 is open on one side and sealed with an end cap 33. There is a liquid inlet pipe 31 and an exhaust pipe 32 on the top, and the liquid inlet pipe 31 is connected to the collecting pipe 25. The chloride purification system provided by this application can purify chloride to 4.5N, greatly improving product quality, meeting the stringent requirements of chemical vapor deposition technology, and effectively solving the problems of reduced quality and unstable performance of deposited films caused by excessive chloride impurities in China. Secondly, the system has a simple structure and consists of a distillation kettle, a reflux assembly, and a receiving tube. Each component has a clear function and can switch between reflux and fractionation operations with one button through a stopcock. It is easy to operate and maintain, reducing the difficulty of using the equipment and the maintenance cost. BRIEF DESCRIPTION OF THE DRAWINGS

[0026] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present application. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative labor.

[0027] Figure 1 A schematic diagram of the structure of a chloride purification system provided in an embodiment of the present application;

[0028] Figure numerals: 1, distillation kettle; 11, feed pipe; 12, gas injection pipe; 13, distillation outlet pipe; 14, groove; 21, first pipeline; 22, second pipeline; 23, third pipeline; 24, fourth pipeline; 25, liquid collecting pipe; 26, stopcock; 27, condensation part; 28, stuffing part; 29, condensation device; 3, receiving pipe; 31, liquid inlet pipe; 32, exhaust pipe; 33, end cover; 4, buffer tank; 41, second air inlet pipe; 42, second air outlet pipe; 5, absorption tank; 51, first air inlet pipe; 52, first air outlet pipe; 6, buffer pipeline. DETAILED DESCRIPTION

[0029] The technical solutions of the embodiments of the present application will be described clearly and completely below in conjunction with the accompanying drawings. Obviously, the described embodiments are part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the specification of the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection requested by the present application.

[0030] In the description of the present application, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicating the orientation or positional relationship, are based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present application. In addition, the terms "first", "second", and "third" are used for descriptive purposes only, and cannot be understood as indicating or implying relative importance.

[0031] Unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection or an indirect connection through an intermediate medium, or it can be the internal communication of two components. For ordinary technicians in this field, the specific meanings of the above terms in this application can be understood according to specific circumstances.

[0032] The sources of all raw materials in the present invention are not particularly limited and can be purchased from the market or prepared according to conventional methods known to those skilled in the art.

[0033] Example 1, see Figure 1 The present invention provides a chloride purification system, comprising a rectification kettle 1, a reflux component 2, and a receiving tube 3.

[0034] The top of the distillation kettle 1 is provided with a feed pipe 11 connected to the outside, a gas injection pipe 12, a distillation gas outlet pipe 13, and a groove 14 formed by the top inwardly concave, which is used to place a thermometer to detect the temperature inside the distillation kettle 1; the feed pipe 11 is also provided with a grinding plug for sealing the feed pipe 11;

[0035] The reflux assembly 2 includes a first pipeline 21 connected to the rectification gas outlet pipe 13, and also includes a second pipeline 22, a third pipeline 23, a fourth pipeline 24, and a liquid collecting pipe 25; wherein the pipe wall of the first pipeline 21 is connected to one end of the second pipeline 22 and the third pipeline 23 to form two three-way branches; the other ends of the second pipeline 22 and the third pipeline 23 are connected to the pipe wall of the fourth pipeline 24 to form two three-way branches; that is, the four three-way branches formed by the second pipeline 22 and the third pipeline 23 connecting the pipe walls of the first pipeline 21 and the fourth pipeline 24 end to end form a quadrilateral loop in series; one end of the liquid collecting pipe 25 is connected to the connection between the second pipeline 22 and the fourth pipeline 24 to form a three-way branch; the liquid collecting pipe 25 is also provided with a cock 26 for controlling the opening and closing state of the liquid collecting pipe 25 to switch the fractionation and reflux operations;

[0036] The reflux assembly 2 further includes a condensation member 27 disposed inside the first pipe 21 and a filler member 28 disposed inside the fourth pipe 24, and the opening or closing state of the pipe wall branches of the first pipe 21 and the fourth pipe 24 is controlled by the up and down movement of the condensation member 27 and the filler member 28;

[0037] The reflux assembly 2 is also provided with a condensing device 29, which is placed outside the tube walls of the first pipe 21, the second pipe 22, the third pipe 23, the fourth pipe 24, and the liquid collecting pipe 25, and provides a temperature difference therefor to condense the steam entering the pipes;

[0038] The receiving tube 3 is a container with an opening on one side, and an end cap 33 is used to seal the opening of the receiving tube 3. A liquid inlet pipe (31) and an exhaust pipe 32 communicating with the outside are also provided at the top of the receiving tube 3. The liquid inlet pipe 31 is connected to the liquid collecting pipe 25 of the reflux assembly 2.

[0039] It should be noted that the feed pipe 11 is used to feed crude chloride into the distillation kettle 1, the gas injection pipe 12 can be used to introduce nitrogen before purification, the distillation outlet pipe 13 is the channel for the chloride to leave the distillation kettle 1 after being heated and evaporated, and the top of the distillation kettle 1 is also provided with an inwardly concave groove 14 for placing a thermometer to monitor the internal temperature of the distillation kettle 1. When the vaporized chloride enters the reflux assembly 2 through the rectification outlet pipe 13, if the stopcock 26 is adjusted to make the collecting pipe 25 in a closed state, the internal pressure of the pipeline gradually increases, so that the condensation member 27 and the filler member 28 move upward to open the pipe wall branch of the first pipe 21 and the fourth pipe 24, and form a quadrilateral passage with the second pipe 22 and the third pipe 23, so that the steam circulates stably in the loop for reflux operation; if the stopcock 26 on the collecting pipe 25 is opened to make the collecting pipe 25 in an open state, the internal pressure of the pipeline decreases accordingly, and the condensation member 27 and the filler member 28 move downward to close the branch connected to the third pipe 23, and the steam condenses through the second pipe 22 and the collecting pipe 25 and flows to the receiving pipe 3, realizing the switch from reflux to fractionation. The receiving pipe 3 is a container with one side open and sealed with an end cap 33, and the end cap 33 can be opened to replace the quartz boat, and the exhaust pipe 32 at the top of the receiving pipe 3 is used to discharge the waste gas generated during the purification process.

[0040] Specifically, the system provided by the present application can be used to purify gallium chloride, indium chloride, antimony chloride, arsenic chloride, aluminum iodide, titanium iodide, molybdenum dichloride, molybdenum tetrachloride, molybdenum pentachloride, tungsten chloride, tungsten oxytetrachloride, and tungsten hexachloride.

[0041] Furthermore, a quartz receiving boat is provided in the receiving tube 3 for receiving the distillate; the end of the liquid inlet tube 31 extends downward to the inside of the receiving tube 3 so that the distillate can flow downward along the liquid inlet tube 31 into the quartz receiving boat.

[0042] It should be noted that, since the end of the liquid inlet pipe 31 extends downward, the distillate can flow directly downward into the quartz receiving boat under the action of gravity. This directional flow ensures that the distillate can be accurately collected in the quartz receiving boat, avoiding the distillate splashing around inside the receiving tube 3 or adhering to the wall of the receiving tube 3, resulting in incomplete collection or loss; the quartz receiving boat is used to receive the distillate, and the quartz receiving boat can be replaced according to different stages (such as the front distillate and middle distillate collection stages) to achieve separate collection of different distillates.

[0043] Furthermore, the lower ends of the condensation piece 27 and the filler piece 28 are provided with barbs, and the upper ends of the first pipe 21 and the fourth pipe 24 protrude into the interior of the pipe to form protruding ends, and the barbs and the protruding ends cooperate with each other to prevent the condensation piece 27 and the filler piece 28 from being sprayed off from the upper ends of the first pipe 21 and the fourth pipe 24 during the operation of the device.

[0044] Furthermore, a funnel is provided at the end of the feed pipe 11 at the top of the distillation kettle 1, so that the raw materials can smoothly enter the feed pipe 11 through the funnel.

[0045] Furthermore, it also includes an absorption tank 5 for containing absorption liquid, and the absorption tank 5 is provided with a first air inlet pipe 51 and a first air outlet pipe 52 ; the first air inlet pipe 51 is connected to the exhaust pipe 32 of the receiving pipe 3 .

[0046] It should be noted that the first air inlet pipe 51 is connected to the second air outlet pipe 42 of the buffer tank 4 to receive the buffered tail gas, and the tail gas contacts the absorption liquid in the absorption tank 5 for preliminary treatment, and the treated gas is discharged from the first air outlet pipe 52, and then further treated by the subsequent spray tower before reaching the emission standard. The absorption tank 5 is set to absorb and treat harmful substances in the tail gas to reduce pollution to the environment.

[0047] Furthermore, it also includes a buffer tank 4, which is arranged between the receiving pipe 3 and the absorption tank 5; a second air inlet pipe 41 and a second air outlet pipe 42 are provided on the top of the buffer tank 4; the second air inlet pipe 41 is connected to the exhaust pipe 32 of the receiving pipe 3; the second air outlet pipe 42 is connected to the first air inlet pipe 51 of the absorption tank 5.

[0048] It should be noted that the second air inlet pipe 41 is connected to the exhaust pipe 32 of the receiving pipe 3 to receive the exhaust gas discharged from the receiving pipe 3, and the second air outlet pipe 42 is connected to the first air inlet pipe 52 of the absorption tank 5 to transport the exhaust gas to the absorption tank 5. The buffer tank 4 can buffer the exhaust gas, so that the exhaust gas can enter the absorption tank 5 more smoothly for treatment. Further, the second air outlet pipe 42 and / or the first air inlet pipe 51 are provided with a cavity.

[0049] Furthermore, at least three cavities are provided.

[0050] It should be noted that by providing a cavity, it can play a role in buffering and stabilizing the airflow when the exhaust gas passes through, which is beneficial for the exhaust gas to more fully contact with the absorption liquid in the absorption tank and improve the absorption efficiency.

[0051] Furthermore, a buffer pipe 6 is provided, the two ends of which are connected to the fourth pipe 24 and the second air intake pipe 41 .

[0052] It should be noted that the buffer pipe 6 plays a role in buffering and stabilizing the airflow.

[0053] Example 2: The present application also provides a method for purifying chloride, which is purified using a chloride purification system, and the specific steps are as follows:

[0054] Step S1, injecting nitrogen into the distillation kettle 1 through the gas injection pipe 12 to empty the distillation kettle 1, and then feeding the crude chloride into the distillation kettle 1 from the feed pipe 11, and covering the grinding plug tightly.

[0055] Step S2, control the stopcock 26 to keep the liquid collecting pipe 25 in a closed state, heat the distillation kettle 1 to 500° C., vaporize the crude chloride and enter the quadrilateral loop from the first pipeline 21 to circulate and reflux for the first period of time;

[0056] Step S3, after the reflux is completed, the stopcock 26 is opened, and the vaporized chloride is first condensed through the liquid collecting pipe 25, and then collected by the quartz boat in the receiving pipe 3 through the liquid inlet pipe 31. This is the collection process of the front fraction; wherein, the collection of the front fraction must meet the following conditions: the collection time is 1.5h or the mass of the collected front fraction accounts for 20% of the mass of the feed;

[0057] Step S4, after the collection of the current fraction is completed, the distillation kettle 1 is heated to raise the temperature by 10° C. The fraction collected at this temperature is a high-purity chlorine compound.

[0058] Specifically, the first period of continuous circulation reflux lasts for 1 hour.

[0059] It should be noted that the gas injection pipe 12 can be used to introduce nitrogen to empty the distillation kettle 1 before purification, creating a pure nitrogen atmosphere for subsequent reactions and avoiding interference of impurities in the chloride purification process. This process cooperates with the feed pipe 11 to ensure that the crude chloride is fed into the emptied distillation kettle 1 under appropriate conditions.

[0060] During the whole operation, the temperature in the reactor should be no less than 500°C. Such a high temperature environment can fully gasify the chloride for subsequent separation and purification operations. When the chloride vapor enters the first pipeline 21, since the cock 26 on the collecting pipe 25 is in a closed state, the internal pressure of the pipeline gradually increases, causing the condensing member 27 and the filling member 28 to move upward to open the pipe wall branch of the first pipeline 21 and the fourth pipeline 24, forming a quadrilateral passage with the second pipeline 22 and the third pipeline 23, so that the steam can circulate stably in the loop. The circulation reflux time is 1 hour. At this time, the chloride is fully mixed and initially separated in the reflux component 2. When the reflux reaches the preset 1h, the stopcock 26 on the collecting pipe 25 is opened, and the internal pressure of the pipe is reduced accordingly. The condensing member 27 and the filling member 28 move downward to close the branch connected to the third pipe 23. At this time, the chloride vapor flows to the receiving pipe 3 after condensation through the second pipe 22 and the collecting pipe 25, realizing the switch from reflux to fractionation; after the current fraction is collected for about 1.5h or accounts for 20% of the feed weight, the stopcock 26 is closed to stop the collection, and then a blank quartz boat is replaced, and the reaction temperature in the distillation kettle 1 is increased at the same time. After the temperature is increased by 10°C, the stopcock 26 is opened again, and the fraction collected at this temperature is a high-purity chlorine compound.

[0061] The purity of the chloride obtained in this embodiment can reach 4.5N, which greatly improves the product quality, meets the stringent requirements of the chemical vapor deposition process, and effectively solves the problems of reduced quality and unstable performance of deposited films caused by the large number of chloride impurities in China. Secondly, the system has a simple structure and consists of a distillation kettle, a reflux assembly and a receiving tube. The functions of each component are clear, and the reflux and fractionation operations can be switched by one button through the cock. It is easy to operate and maintain, reducing the difficulty of using the equipment and the maintenance cost.

[0062] The above are only preferred embodiments of the present application and are not intended to limit the present invention. Although the present application has been described in detail with reference to the examples, those skilled in the art can still modify the technical solutions recorded in the aforementioned examples or make equivalent substitutions for some of the technical features therein. However, any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.

Claims

1. A chloride purification system, characterized in that: It comprises a distillation kettle (1), a reflux component (2), and a receiving pipe (3). The top of the distillation kettle (1) is provided with a feed pipe (11) communicating with the outside, a gas injection pipe (12), a distillation gas outlet pipe (13), and a groove (14) formed by the top being recessed inwardly and used for placing a thermometer to detect the temperature inside the distillation kettle (1); the feed pipe (11) is also provided with a grinding plug for sealing the feed pipe (11); The reflux assembly (2) comprises a first pipeline (21) connected to a rectification gas outlet pipe (13), and further comprises a second pipeline (22), a third pipeline (23), a fourth pipeline (24), and a liquid collecting pipe (25); the second pipeline (22) and the third pipeline (23) are both connected end to end to the pipe walls of the first pipeline (21) and the fourth pipeline (24) to form a quadrilateral loop; one end of the liquid collecting pipe (25) is connected to the connection between the second pipeline (22) and the fourth pipeline (24) to form a three-way branch; the liquid collecting pipe (25) is also provided with a cock (26) for controlling the opening and closing state of the liquid collecting pipe (25) to switch between fractionation and reflux operations; The reflux assembly (2) further comprises a condensing member (27) arranged inside the first pipe (21), and a filling member (28) arranged inside the fourth pipe (24), and the opening or closing state of the pipe wall branches of the first pipe (21) and the fourth pipe (24) is controlled by the up and down movement of the condensing member (27) and the filling member (28); The reflux assembly (2) is further provided with a condensing device (29), and the condensing device (29) is used to condense the steam entering the first pipe (21), the second pipe (22), the third pipe (23), the fourth pipe (24), and the liquid collecting pipe (25); The receiving tube (3) is a container with an opening on one side, and an end cover (33) is used to seal the opening of the receiving tube (3); a liquid inlet pipe (31) and an exhaust pipe (32) communicating with the outside are also provided at the top of the receiving tube (3), and the liquid inlet pipe (31) is connected to the liquid collecting pipe (25) of the reflux assembly (2).

2. The chloride purification system according to claim 1, characterized in that: The receiving tube (3) is provided with a quartz receiving boat for receiving the distillate; The end of the liquid inlet pipe (31) extends downward to the interior of the receiving pipe (3), so that the distillate can flow downward along the liquid inlet pipe (31) into the quartz receiving boat.

3. The chloride purification system according to claim 1, characterized in that: The lower ends of the condensing member (27) and the filling member (28) are both provided with barbs, and the upper ends of the first pipe (21) and the fourth pipe (24) are both protruded toward the inside of the pipe to form protruding ends, and the barbs and the protruding ends cooperate with each other to prevent the condensing member (27) and the filling member (28) from being ejected from the upper ends of the first pipe (21) and the fourth pipe (24) during the operation of the device.

4. The chloride purification system according to claim 1, characterized in that: A funnel is provided at the end of the feed pipe (11) at the top of the rectification kettle (1), so that the raw materials can smoothly enter the feed pipe (11) through the funnel.

5. The chloride purification system according to claim 1, characterized in that: It also comprises an absorption tank (5) for containing absorption liquid, the absorption tank (5) being provided with a first air inlet pipe (51) and a first air outlet pipe (52); the first air inlet pipe (51) is connected to the air outlet pipe (32) of the receiving pipe (3).

6. The chloride purification system according to claim 5, characterized in that: It also comprises a buffer tank (4) arranged between the receiving pipe (3) and the absorption tank (5); a second air inlet pipe (41) and a second air outlet pipe (42) are arranged on the top of the buffer tank (4); the second air inlet pipe (41) is connected to the exhaust pipe (32) of the receiving pipe (3); and the second air outlet pipe (42) is connected to the first air inlet pipe (51) of the absorption tank (5).

7. The chloride purification system according to claim 6, characterized in that: The second air outlet pipe (42) and / or the first air inlet pipe (51) is provided with a cavity.

8. The chloride purification system according to claim 7, characterized in that: At least 3 cavities are provided.

9. The chloride purification system according to claim 6, characterized in that: A buffer pipe (6) is also provided, the two ends of which are connected to the fourth pipe (24) and the second air inlet pipe (41).

10. A method for purifying chloride, characterized in that: The purification is carried out using the chloride purification system according to any one of claims 1 to 9, and the specific steps are as follows: Step S1, injecting nitrogen into the distillation kettle (1) through the gas injection pipe (12) to empty the distillation kettle (1), then feeding the crude chloride into the distillation kettle (1) from the feed pipe (11), and tightly covering the grinding plug; Step S2, controlling the stopcock (26) to keep the liquid collecting pipe (25) in a closed state, heating the distillation kettle (1) to 500° C., vaporizing the crude chloride and allowing it to enter the quadrilateral loop through the first pipeline (21) for a first period of time; Step S3, after the reflux is completed, the stopcock (26) is opened, and the vaporized chloride is first condensed through the liquid collecting pipe (25), and then collected by the quartz boat in the receiving pipe (3) through the liquid inlet pipe (31). This is the collection process of the front fraction; wherein the collection of the front fraction must meet the following conditions: the collection time is 1.5 hours or the mass of the collected front fraction accounts for 20% of the mass of the feed; Step S4, when the collection of the current fraction is completed, the distillation kettle (1) is heated to raise the temperature by 10° C. The fraction collected at this temperature is a high-purity chlorine compound.

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