A continuous receiving device for negative pressure rectification of heat-sensitive materials

Abstract

The utility model provides a kind of for heat-sensitive material's negative pressure rectification continuous receiving device, including receiving tank subassembly and product storage tank subassembly, the top of receiving tank subassembly is connected with multi-way reversing valve, the multi-way reversing valve is connected with rectifying column, the bottom of receiving tank subassembly is connected with product storage tank subassembly, sampling port is equipped between the receiving tank subassembly with the product storage tank subassembly, wherein, the receiving tank subassembly includes 2 or more parallel receiving tank;The receiving tank is equipped with vent valve, for communicating with atmosphere;The receiving tank is equipped with discharge valve, for being connected with product storage tank subassembly;The receiving tank and the product storage tank subassembly are equipped with vacuum valve, for being connected with vacuum system.The above-mentioned device realizes the continuous collection of heat-sensitive material, reduces rectifying column pressure fluctuation, improves separation efficiency, simultaneously avoids the problem such as leakage and impurity caused by external power device.

Description

Technical Field

[0001] This utility model belongs to the field of chemical process equipment technology, and relates to the field of separation technology of heat-sensitive materials, specifically to a negative pressure distillation continuous receiving device for heat-sensitive materials. Background Technology

[0002] Thermosensitive materials are a class of materials that are unstable when heated. They are prone to decomposition, polymerization, oxidation and other deterioration reactions when heated. For example, some organosilicon monomers or pharmaceutical intermediates are highly thermosensitive. At the same time, thermosensitive materials are also characterized by high boiling points, difficulty in separation and high viscosity. Thermosensitive materials cannot be evaporated under normal atmospheric pressure. Therefore, in industrial applications, when distilling and purifying thermosensitive materials, it is necessary to change the pressure by drawing a vacuum to lower their boiling points.

[0003] Existing negative pressure distillation systems typically consist of raw material tanks, membrane evaporators, distillation columns, collection tanks, condensers, and vacuum pumps. For heat-sensitive materials, the collection tanks in negative pressure distillation often operate intermittently in single tanks, preventing continuous product reception. Furthermore, when sampling using intermittent single-tank operation, the system needs to break the vacuum, leading to pressure fluctuations (±0.02 MPa) in the distillation column, affecting separation efficiency. Additionally, the liquid transfer process relies on external power units (such as transfer pumps) to complete material transfer, making it impossible to automate flow using the system's own pressure, and external power units are prone to leakage and introducing impurities. Utility Model Content

[0004] Therefore, the technical problem to be solved by this utility model is to provide a negative pressure distillation continuous receiving device for heat-sensitive materials, so as to realize the continuous collection of heat-sensitive materials, reduce pressure fluctuations in the distillation column, improve separation efficiency, and at the same time, use the system's own pressure to realize product flow, avoiding problems such as leakage and impurities caused by using external power devices.

[0005] To achieve the above objectives, this utility model provides the following technical solution:

[0006] This utility model provides a negative pressure distillation continuous receiving device for heat-sensitive materials, which includes a receiving tank assembly 1 and a product storage tank assembly 2. The top of the receiving tank assembly 1 is connected to a multi-way reversing valve 3, the multi-way reversing valve 3 is connected to a distillation column 4, the bottom of the receiving tank assembly 1 is connected to the product storage tank assembly 2, and a sampling port 5 is provided between the receiving tank assembly 1 and the product storage tank assembly 2.

[0007] The receiving tank assembly 1 includes two or more receiving tanks connected in parallel;

[0008] Each receiving tank is equipped with a vent valve for communicating with the atmosphere;

[0009] Each receiving tank is equipped with a discharge valve for connecting to the product storage tank assembly 2.

[0010] Both the receiving tank and the product storage tank assembly 2 are equipped with vacuum valves for connection to a vacuum system.

[0011] In some embodiments of this utility model, a condenser 7 is provided between the distillation column 4 and the multi-way reversing valve 3.

[0012] In some embodiments of this utility model, an intermediate storage tank 8 is provided between the multi-way reversing valve 3 and the condenser 7, wherein the intermediate storage tank 8 is also connected to the top of the distillation column 4.

[0013] In some embodiments of this utility model, a filter 6 is provided between the receiving tank assembly 1 and the product storage tank assembly 2.

[0014] In some embodiments of this utility model, the filter 6 adopts a double-layer filter element structure, wherein the outer filter element has a pore size of 5-10μm and the inner filter element has a pore size of 0.1-1μm.

[0015] In some embodiments of this utility model, the receiving tank assembly 1 includes three receiving tanks connected in parallel, and the multi-way reversing valve 3 is a four-way valve.

[0016] In some embodiments of this utility model, the product storage tank assembly 2 includes two product tanks, wherein each product tank is equipped with a vent valve and a feed valve.

[0017] In some embodiments of this utility model, the receiving tank is further provided with a demetallizing resin bed 10, wherein the demetallizing resin is a chelating resin.

[0018] In some embodiments of this utility model, the volume of the receiving tank is 80-120L, and the height-to-diameter ratio is 1.5-2.5:1;

[0019] The chelating resin has a packing height of 400-600 mm, a particle size of 0.3-0.5 mm, and a wet apparent density of 700-740 kg / m³. 3 .

[0020] In some embodiments of this utility model, the vacuum valves are all pneumatic valves, and the receiving tank has a built-in pressure sensing module.

[0021] Both the pressure sensing module and the vacuum valve are electrically connected to the controller.

[0022] Beneficial effects:

[0023] This invention connects multiple receiving tanks in parallel to the product storage tank assembly, and combines the vacuum valve, vent valve, and discharge valve of the receiving tanks to achieve continuous receiving of distilled products. Furthermore, the sampling port can be disconnected from the distillation column system during sampling, reducing pressure fluctuations in the distillation column system and improving separation efficiency. During liquid transfer, the liquid can be automatically transferred using its own pressure, avoiding problems such as sample leakage and the introduction of impurities caused by the introduction of external power devices. Attached Figure Description

[0024] To make the content of this utility model easier to understand, the present utility model will be further described in detail below with reference to specific embodiments and accompanying drawings.

[0025] Figure 1 This is a schematic diagram of the negative pressure distillation continuous receiving device for heat-sensitive materials according to this utility model.

[0026] The annotations in the attached figures are explained as follows:

[0027] 1-Receiving tank assembly, 11-First receiving tank, 12-Second receiving tank, 13-Third receiving tank, 2-Product storage tank assembly, 21-First product tank, 22-Second product tank, 3-Multi-way reversing valve, 4-Distillation column, 5-Sampling port, 6-Filter, 7-Condenser, 8-Intermediate storage tank, 911-Vacuum valve of first receiving tank, 912-Vacuum valve of second receiving tank, 913-Vacuum valve of third receiving tank, 914-Vacuum valve of first product tank, 915 - Vacuum valve for the second product tank; 921 - Discharge valve for the first receiving tank; 922 - Discharge valve for the second receiving tank; 923 - Discharge valve for the third receiving tank; 924 - Feed valve for the first product tank; 925 - Feed valve for the second product tank; 931 - Vent valve for the first receiving tank; 932 - Vent valve for the second receiving tank; 933 - Vent valve for the third receiving tank; 934 - Vent valve for the first product tank; 935 - Vent valve for the second product tank; 10 - Demetallized resin bed. Detailed Implementation

[0028] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present utility model are within the protection scope of the present utility model.

[0029] On the one hand, in one specific embodiment of this application, this application provides a negative pressure distillation continuous receiving device for heat-sensitive materials to solve at least one of the following problems existing in the prior art: ① The system needs to break the vacuum during sampling, resulting in pressure fluctuations (±0.02MPa) in the distillation column, affecting the separation efficiency; ② The liquid transfer process relies on an external power device (such as a transfer pump) to complete the material transfer, and it is impossible to achieve automated flow by relying on the system's own pressure, and the external power device is prone to leakage and introduction of impurities; ③ Metal impurities (such as Fe) 3+ Al 3+ ) It is easy for impurities to enter the product tank with the material, affecting the product purity (actual impurity content ≥5ppm); ④ Manual valve switching takes ≥3 minutes / time, resulting in 5-8% material thermal decomposition loss. The following will describe the negative pressure distillation continuous receiving device for heat-sensitive materials with reference to the attached diagram.

[0030] Specifically, the negative pressure distillation continuous receiving device for heat-sensitive materials provided in this application embodiment is exemplified by, for example, the following reference: Figure 1 As shown, a negative pressure distillation continuous receiving device for heat-sensitive materials includes a receiving tank assembly 1 and a product storage tank assembly 2. The top of the receiving tank assembly 1 is connected to a multi-way reversing valve 3, which is connected to a distillation column 4. The bottom of the receiving tank assembly 1 is connected to the product storage tank assembly 2. A sampling port 5 is provided between the receiving tank assembly 1 and the product storage tank assembly 2. The receiving tank assembly 1 includes two or more receiving tanks connected in parallel. Each receiving tank is equipped with a vent valve for communicating with the atmosphere. Each receiving tank is equipped with a discharge valve for connecting to the product storage tank assembly 2. Both the receiving tanks and the product storage tank assembly 2 are equipped with vacuum valves for connecting to a vacuum system.

[0031] It should be noted that the multi-way directional valve in this application can be a single directional valve, such as a three-way valve, a four-way valve, a five-way valve, etc.; or it can be a combination of multiple directional valves. For example, a combination of two three-way valves in series can achieve one inlet and three outlets, controlling the distillation column to be connected to one receiving tank at a time, thereby realizing the continuous collection of distillation products.

[0032] When receiving distillation products begins, close the discharge valves of all receiving tanks, open the vacuum valves of all receiving tanks to evacuate, and adjust the multi-way reversing valve 3 to connect one receiving tank in receiving tank assembly 1 to distillation column 4. The receiving tank connected to the distillation column begins receiving distillation products. When sampling is required, adjust the multi-way reversing valve 3 to connect another receiving tank in receiving tank assembly 1 to distillation column 4, close the vacuum valve of the previous receiving tank, open its vent valve to vent, and then open the discharge valve below it to take a sample from sampling port 5. After sampling, close the discharge valve and vent valve, open the vacuum valve to evacuate to the required pressure, such as -0.08 to -0.1 MPa, and then adjust the multi-way reversing valve 3 to switch to that receiving tank to continue receiving distillation products.

[0033] When the liquid level in the receiving tank reaches the set standard level, for example, 80-90% of the maximum level, the multi-way reversing valve 3 is adjusted to connect another receiving tank in receiving tank assembly 1 to the distillation column 4, continuing to receive distilled products. The vacuum valve of the previous receiving tank is closed, and the vent valve and discharge valve of the previous receiving tank are opened. The vacuum valve of product storage tank assembly 2 is opened, and the distilled products automatically flow into product storage tank assembly 2 under pressure. After the discharge is completed, the vacuum valve of product storage tank assembly 2 is closed, the vent valve and discharge valve of the receiving tank are closed, and the vacuum valve is opened to evacuate to the required pressure for standby. This process is repeated for multiple receiving tanks, allowing for the sequential receipt of distilled products and discharge to the product tank, achieving continuous receiving of distilled products. Simultaneously, it ensures that the pressure of the distillation column is not affected during sampling, and that the transfer of distilled products can be achieved without external power, avoiding leakage and impurities associated with using external power devices.

[0034] In some embodiments of this utility model, the thermosensitive material includes organosilicon monomers or pharmaceutical intermediates, wherein the boiling point of the thermosensitive material is ≤400℃ and the thermal decomposition temperature of the thermosensitive material is <250℃.

[0035] In some embodiments of this utility model, the product storage tank assembly 2 includes one or more product tanks connected in parallel, and each product tank is equipped with a vacuum valve. In some embodiments of this utility model, the product storage tank assembly 2 includes two product tanks.

[0036] In some embodiments of this utility model, the product can is provided with a vent valve.

[0037] In some embodiments of this utility model, a feed valve is provided between the product tank and the receiving tank assembly 1 for connecting to the receiving tank assembly.

[0038] In some embodiments of this utility model, the receiving tank assembly 1 includes three receiving tanks connected in parallel, and the multi-way reversing valve 3 is a four-way valve.

[0039] In some embodiments of this utility model, a condenser 7 is provided between the distillation column 4 and the multi-way reversing valve 3.

[0040] In some embodiments of this utility model, an intermediate storage tank 8 is provided between the multi-way reversing valve 3 and the condenser 7, wherein the intermediate storage tank 8 is also connected to the top of the distillation column 4 through a reflux pipe.

[0041] In some embodiments of this invention, a filter 6 is provided between the receiving tank assembly 1 and the product storage tank assembly 2. In some embodiments of this invention, the filter 6 adopts a double-layer filter element structure, wherein the filter element is made of polytetrafluoroethylene (PTFE), the outer filter element has a pore size of 5-10 μm, and the inner filter element has a pore size of 0.1-1 μm. The 5-10 μm outer filter element intercepts large particles, while the 0.1-1 μm inner filter element adsorbs fine impurities, thereby reducing the risk of inner layer clogging and extending the filter element's lifespan.

[0042] In some embodiments of this invention, the receiving tank further includes a demetallizing resin bed 10, wherein the demetallizing resin is a chelating resin. In some embodiments, the receiving tank has a volume of 80-120L and a height-to-diameter ratio of 1.5-2.5:1; the filling height of the chelating resin is 400-600mm, the particle size of the chelating resin is 0.3-0.5mm, and the wet apparent density of the chelating resin is 700-740kg / m³. 3 .

[0043] It should be noted that the type and source of the chelating resin are not limited as long as the purpose of this utility model can be achieved. For example, it can be D401 chelating resin purchased from Langfang Senate Chemical Co., Ltd. The distillation product passes through a metal removal resin bed to remove metal impurities (e.g., Fe) from the product. 3+ Al 3+ (etc.), improving product purity. Furthermore, the above structure enhances ion exchange efficiency, resulting in a higher removal rate of metal impurities, reaching over 98%, including Fe. 3+ Content < 2 ppm.

[0044] In some embodiments of this utility model, the vacuum valves in the above-mentioned device are all pneumatic valves, and the receiving tank is also equipped with a pressure sensing module. Both the pressure sensing module and the vacuum valves are electrically connected to the controller. The pressure of the distillation column is tested by the pressure sensing module, and the controller controls the corresponding actuators to control the pressure fluctuations in the distillation column, such as controlling the opening degree of the vacuum valve, thereby improving separation efficiency. The feed valve, discharge valve, and multi-way directional valve can also be pneumatic valves, enabling automatic opening and closing of the valves, avoiding the time-consuming problem of manual valve switching, and reducing material thermal decomposition losses.

[0045] It should be noted that the pressure sensing module of this utility model is not particularly limited, as long as it can realize pressure testing, for example, it can be a pressure sensor.

[0046] On the other hand, this application also provides a negative pressure distillation system including the above-mentioned continuous receiving device, which includes a distillation column 4, a condenser 7, an intermediate storage tank 8, a receiving tank assembly 1 and a product storage tank assembly 2 connected in sequence.

[0047] A multi-way reversing valve 3 is provided between the top of the receiving tank assembly 1 and the intermediate storage tank 8, and a sampling port 5 is provided between the receiving tank assembly 1 and the product storage tank assembly 2.

[0048] The receiving tank assembly 1 includes two or more receiving tanks connected in parallel; each receiving tank is equipped with a vent valve for communicating with the atmosphere; each receiving tank is equipped with a discharge valve for connecting to the product storage tank assembly 2; both the receiving tank and the product storage tank assembly 2 are equipped with vacuum valves for connecting to a vacuum system.

[0049] In some specific embodiments of this utility model, please refer to [link / reference]. Figure 1As shown, the product outlet of distillation column 4 is connected to one end of condenser 7 via a pipeline, and the other end of condenser 7 is connected to intermediate storage tank 8 via a pipeline. Intermediate storage tank 8 is connected to the top of distillation column 4 via a reflux pipeline, and the bottom of intermediate storage tank 8 is connected to a first receiving tank 11, a second receiving tank 12, and a third receiving tank 13 connected in parallel via pipelines. A multi-way directional valve 3 is installed on the pipeline connecting intermediate storage tank 8 to the first receiving tank 11, the second receiving tank 12, and the third receiving tank 13 in parallel to control the flow of distilled products into the first receiving tank 11, the second receiving tank 12, and the third receiving tank 13. A receiving tank 11, a second receiving tank 12, or a third receiving tank 13 is provided. At the bottom of each receiving tank, a first receiving tank discharge valve 921, a second receiving tank discharge valve 922, and a third receiving tank discharge valve 923 are respectively provided. These valves are connected in parallel via pipes and then connected to one end of a filter 6 via another pipe. A first product tank 21 and a second product tank 22 are respectively provided with... A product tank inlet valve 924 and a second product tank inlet valve 925 are connected in parallel via a pipeline and then connected to the other end of a filter 6 via another pipeline. A sampling port 5 is provided on the pipeline connecting the filter 6 to the parallel first product tank 21 and the second product tank 22. The first receiving tank 11 is provided with a first receiving tank vacuum valve 911 and a first receiving tank vent valve 931. The second receiving tank 12 is provided with a second receiving tank vacuum valve 912 and a second receiving tank vent valve 932. The third receiving tank 13 is provided with a third receiving tank vacuum valve 913 and a third receiving tank vent valve 933. The first product tank 21 is provided with a first product tank vacuum valve 914 and a first product tank vent valve 934. The second product tank 22 is provided with a second product tank vacuum valve 915 and a second product tank vent valve 935. The first receiving tank 11, the second receiving tank 12, the third receiving tank 13, the first product tank 21, and the second product tank 22 are connected to a vacuum system via vacuum valves.

[0050] The technical effects of the negative pressure distillation continuous receiving device for heat-sensitive materials of this utility model will be specifically described below through specific embodiments. In the embodiments, all original reagents and instruments are commercially available, and experimental methods without specific conditions are conventional methods and conditions well known in the art, or according to the conditions recommended by the instrument manufacturer.

[0051] Example 1

[0052] See Figure 1 In this embodiment, the filter 6 is used in a negative pressure distillation continuous receiving device for heat-sensitive materials. The filter 6 adopts a double-layer filter element structure. Both filter elements are made of polytetrafluoroethylene (PTFE). The outer filter element has a pore size of 10μm, and the inner filter element has a pore size of 0.5μm.

[0053] The first, second, and third receiving tanks each have a volume of 100L, a height-to-diameter ratio of 2:1, and are made of 316L stainless steel. Each tank is equipped with a pressure sensor (range -0.1 to 0.5MPa, accuracy ±0.5%FS), and the pressure sensor is electrically connected to the controller.

[0054] Condenser 7 is a shell-and-tube condenser, in which the tube side carries the distillation product and the shell side carries the cooling medium.

[0055] Multi-way directional valve 3 is a four-way valve.

[0056] The filling height of the metal removal resin bed 10 is 500 mm. The metal removal resin is D401 chelating resin (wet apparent density of 700-740 kg / m³) purchased from Langfang Senate Chemical Co., Ltd. 3 (Particle size is 0.5 mm).

[0057] The vacuum valve, the vent valve, the receiving tank discharge valve, the product tank inlet valve, and the multi-way reversing valve are all pneumatic threaded valves (response time <1s). The above-mentioned pneumatic threaded valves are all electrically connected to the controller to realize automatic valve control.

[0058] This device is used to receive the pharmaceutical intermediate 2-chloro-5-trifluoromethylpyridine (boiling point 215℃). During operation, the multi-way reversing valve 3 is adjusted to connect the first receiving tank 11 to the intermediate storage tank 8. The discharge valves of all receiving tanks are closed, and the vacuum valves of all receiving tanks are opened to evacuate to a pressure of -0.085 MPa. The top product of the distillation column (2-chloro-5-trifluoromethylpyridine) enters the first receiving tank at a flow rate of 200 L / h. When sampling is required, the multi-way reversing valve 3 is adjusted to connect the second receiving tank... The receiving tank 12 is connected to the distillation column 4. The vacuum valve 911 of the first receiving tank is closed, and the vent valve 931 of the first receiving tank is opened to vent. Then, the discharge valve 921 of the first receiving tank below is opened, and a sample is taken from the sampling port 5. After the sampling is completed, the discharge valve 921 and the vent valve 931 of the first receiving tank are closed, and the vacuum valve 911 of the first receiving tank is opened to evacuate to a pressure of -0.085MPa. Then, the multi-way reversing valve 3 is adjusted to switch to the first receiving tank 11 to continue receiving the distillation product.

[0059] When the liquid level in the first receiving tank 11 reaches 80% of the maximum liquid level, the distillation product stays in the demetallized resin bed for about 15 minutes. Adjust the multi-way reversing valve 3 to connect the second receiving tank 12 with the distillation column 4 to continue receiving the distillation product. Close the vacuum valve 911 of the first receiving tank, open the vent valve 931 and the discharge valve 921 of the first receiving tank, and open the vacuum valve 914 and the feed valve 924 of the first product tank. The distillation product flows automatically from the first receiving tank 11 into the first product tank 21 under pressure. After the liquid is discharged, close the vacuum valve 914 and the feed valve 924 of the first product tank, close the vent valve 931 and the discharge valve 921 of the first receiving tank, and open the vacuum valve 911 of the first receiving tank to evacuate to a pressure of -0.085MPa for standby.

[0060] When the liquid level in the second receiving tank 11 reaches 80% of the maximum liquid level, adjust the multi-way reversing valve 3 to connect the third receiving tank 13 with the distillation column 4 to continue receiving distilled products; close the vacuum valve 912 of the second receiving tank, open the vent valve 932 of the second receiving tank and the discharge valve 922 of the second receiving tank, open the vacuum valve 914 and the feed valve 924 of the first product tank, and the distilled products will automatically flow from the second receiving tank 12 into the first product storage tank 21 under pressure. After the liquid discharge is completed, close the vacuum valve 914 and the feed valve 924 of the first product tank, close the vent valve 932 of the second receiving tank and the discharge valve 922 of the second receiving tank, open the vacuum valve 912 of the second receiving tank to evacuate to a pressure of -0.085MPa for standby.

[0061] When the liquid level in the third receiving tank 13 reaches 80% of the maximum liquid level, the multi-way reversing valve 3 is adjusted to connect the first receiving tank 13 with the distillation column 4 to continue receiving distilled products. This process is repeated to achieve continuous receiving of distilled products.

[0062] Tests showed that when switching from the first receiving tank 11 to the second receiving tank 12, the pressure fluctuation of the distillation column was only ±0.005 MPa, which is nearly 80% lower than the pressure fluctuation of traditional single-tank intermittent operation. The system has high energy efficiency and can optimize heat transfer through rapid valve response.

[0063] After 72 hours of continuous operation, the product was tested, and the total amount of metal impurities was <5ppm, and the proportion of thermal decomposition products was <0.3%.

[0064] Experiment Example 2

[0065] See Figure 1 In this embodiment, the filter 6 is used in a negative pressure distillation continuous receiving device for heat-sensitive materials. The filter 6 adopts a double-layer filter element structure. Both filter elements are made of polytetrafluoroethylene (PTFE). The outer filter element has a pore size of 10μm, and the inner filter element has a pore size of 0.5μm.

[0066] The first, second, and third receiving tanks each have a volume of 100L, a height-to-diameter ratio of 2:1, and are made of 316L stainless steel. Each tank is equipped with a pressure sensor (range -0.1 to 0.5MPa, accuracy ±0.5%FS), and the pressure sensor is electrically connected to the controller.

[0067] Condenser 7 is a shell-and-tube condenser, in which the tube side carries the distillation product and the shell side carries the cooling medium.

[0068] Multi-way directional valve 3 is a four-way valve.

[0069] The filling height of the metal removal resin bed 10 is 500 mm. The metal removal resin is D401 chelating resin (wet apparent density of 700-740 kg / m³) purchased from Langfang Senate Chemical Co., Ltd. 3 (Particle size is 0.5 mm).

[0070] The vacuum valve, the vent valve, the receiving tank discharge valve, the product tank inlet valve, and the multi-way reversing valve are all pneumatic threaded valves (response time <1s). The above-mentioned pneumatic threaded valves are all electrically connected to the controller to realize automatic valve control.

[0071] This device is used to receive the precursor material tetraethoxysilane (boiling point 168°C). The working process is the same as in Example 1, except that the top material of the distillation column (tetraethoxysilane) enters the receiving tank at a flow rate of 180 L / h, and the distillation product stays in the demetallized resin bed for 20 minutes.

[0072] Experimental results show that when switching from the first receiving tank 11 to the second receiving tank 12, the pressure fluctuation of the distillation column is only ±0.005MPa, which is nearly 80% lower than the pressure fluctuation of traditional single-tank intermittent operation; after 72 hours of continuous operation, the product was tested and found that the total amount of metal impurities was <0.5ppm and the proportion of thermal decomposition products was <0.1%.

[0073] In this utility model, unless otherwise explicitly specified and limited, the terms "installation," "connection," "joining," and "fixing," etc., should be interpreted broadly. For example, they can refer to a fixed connection, a detachable connection, or an integral part; they can refer to a mechanical connection or an electrical connection; they can refer to a direct connection or an indirect connection through an intermediate medium; they can refer to the internal communication of two components or the interaction between two components, unless otherwise explicitly limited. Those skilled in the art can understand the specific meaning of the above terms in this utility model according to the specific circumstances.

[0074] In this utility model, unless otherwise explicitly specified and limited, "above" or "below" the second feature can mean that the first feature is in direct contact with the second feature, or that the first feature is in indirect contact with the second feature through an intermediate medium. Furthermore, "above," "on top of," and "over" the second feature can mean that the first feature is directly above or diagonally above the second feature, or simply that the first feature is at a higher horizontal level than the second feature. "Below," "below," and "under" the second feature can mean that the first feature is directly below or diagonally below the second feature, or simply that the first feature is at a lower horizontal level than the second feature.

[0075] In this utility model, if it is described that the first, second, and third are only for the purpose of distinguishing technical features, and should not be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated or the order of the technical features indicated.

[0076] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

[0077] In the description of this specification, the references to terms such as "one embodiment," "some embodiments," "example," "specific example," or "some examples," etc., indicate that a specific feature, structure, material, or characteristic described in connection with that embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

[0078] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the protection scope of this invention.

Claims

1. A continuous receiving device for negative pressure distillation of heat-sensitive materials, characterized in that, The negative pressure distillation continuous receiving device includes a receiving tank assembly (1) and a product storage tank assembly (2). The top of the receiving tank assembly (1) is connected to a multi-way reversing valve (3), and the multi-way reversing valve (3) is connected to a distillation column (4). The bottom of the receiving tank assembly (1) is connected to the product storage tank assembly (2). A sampling port (5) is provided between the receiving tank assembly (1) and the product storage tank assembly (2). The receiving tank assembly (1) includes two or more receiving tanks connected in parallel; Each receiving tank is equipped with a vent valve for communicating with the atmosphere; Each receiving tank is equipped with a discharge valve for connecting to the product storage tank assembly (2); Both the receiving tank and the product storage tank assembly (2) are equipped with vacuum valves for connection to a vacuum system.

2. The negative pressure distillation continuous receiving device for heat-sensitive materials according to claim 1, characterized in that, A condenser (7) is provided between the distillation column (4) and the multi-way reversing valve (3).

3. The negative pressure distillation continuous receiving device for heat-sensitive materials according to claim 2, characterized in that, An intermediate storage tank (8) is provided between the multi-way reversing valve (3) and the condenser (7), wherein the intermediate storage tank (8) is also connected to the top of the distillation column (4).

4. The negative pressure distillation continuous receiving device for heat-sensitive materials according to claim 1, characterized in that, A filter (6) is provided between the receiving tank assembly (1) and the product storage tank assembly (2).

5. The negative pressure distillation continuous receiving device for heat-sensitive materials according to claim 4, characterized in that, The filter (6) adopts a double-layer filter element structure, wherein the outer filter element has a pore size of 5-10μm and the inner filter element has a pore size of 0.1-1μm.

6. The negative pressure distillation continuous receiving device for heat-sensitive materials according to claim 1, characterized in that, The receiving tank assembly (1) includes three receiving tanks connected in parallel, and the multi-way reversing valve (3) is a four-way valve.

7. The negative pressure distillation continuous receiving device for heat-sensitive materials according to claim 1, characterized in that, The product storage tank assembly (2) includes two product tanks, wherein each product tank is equipped with a vent valve and a feed valve.

8. The negative pressure distillation continuous receiving device for heat-sensitive materials according to claim 1, characterized in that, The receiving tank also has a built-in demetallization resin bed (10), wherein the demetallization resin is a chelating resin.

9. The negative pressure distillation continuous receiving device for heat-sensitive materials according to claim 8, characterized in that, The receiving tank has a volume of 80-120L and a height-to-diameter ratio of 1.5-2.5:1; The chelating resin has a packing height of 400-600 mm, a particle size of 0.3-0.5 mm, and a wet apparent density of 700-740 kg / m³. 3 .

10. The negative pressure distillation continuous receiving apparatus for heat-sensitive materials according to any one of claims 1-9, characterized in that, All vacuum valves are pneumatic valves, and the receiving tank has a built-in pressure sensing module. Both the pressure sensing module and the vacuum valve are electrically connected to the controller.

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