Crystallization device

Abstract

The utility model discloses a crystallization device which comprises a mother liquor tank, an oscillation temperature crystallization pipe and a crystallization tank, the oscillation temperature crystallization pipe comprises a plurality of low-temperature crystallization pipes and a plurality of high-temperature crystal dissolving pipes, the plurality of low-temperature crystallization pipes and the plurality of high-temperature crystal dissolving pipes are alternately connected, and the low-temperature crystallization pipes are arranged at the heads and the tails of the low-temperature crystallization pipes, and the mother liquor tank is connected with the first low-temperature crystallization pipe in the oscillation temperature crystallization pipe; and the crystallization tank is connected with the last low-temperature crystallization pipe in the oscillation temperature crystallization pipes. According to the crystallization device provided by the embodiment of the utility model, mother liquor to be crystallized is finally converged to the crystallization tank from the mother liquor tank through the oscillation temperature crystallization pipes of the low-temperature crystallization pipes and the high-temperature crystal dissolving pipes which are alternately arranged, and the mother liquor to be crystallized can be continuously and sequentially cooled and heated by utilizing the device, and is crystallized by utilizing the oscillation temperature; and crystalline substances can be rapidly obtained.

Description

Technical Field

[0001] The utility model relates to the field of crystallization devices, in particular to a crystallization device. Background Art

[0002] Crystallization is a key unit operation in chemical processes and a crucial step in the production of chemical products. It is not only used in the production of certain chemical products, but also has a wide range of applications in product separation, purification, and other aspects. The general crystallization process can be divided into the following sub-processes: solution supersaturation, crystal nucleation in the solution, and growth of the nucleus to a discernible size. Both nucleation and nucleus growth are driven by solution supersaturation. The actual industrial crystallization process can also be divided into these three sub-processes. However, unlike single crystal cultivation, the industrial crystallization process requires greater consideration of fluid dynamics and crystallization kinetics, and to a certain extent, the influence of heat and mass transfer processes.

[0003] Once the crystallization mother liquor in a critical state is stimulated by environmental changes, it is easy to undergo explosive nucleation, thereby obtaining a large amount of fine powder. These powders have a very large specific surface area, resulting in poor stability and easy adsorption of solvents or impurities, which has many adverse effects on the purification, storage, and use of the product. The so-called oscillating temperature crystallization is a process that promotes the Oswald ripening of crystals by heating-cooling cycles at a certain frequency, so that smaller crystals dissolve and grow around larger crystals. It is often used for substances that are easy to precipitate in the form of amorphous flocs or fine powders. The traditional use of oscillating temperature crystallization is to first cool down the crystallization container until crystals precipitate, and then slightly increase the temperature to dissolve the fine powder and recrystallize it on the larger crystals. The above operation needs to be repeated until the crystal size reaches the desired level step by step. Utility Model Content

[0004] Based on this, in order to realize uninterrupted sequential cooling and heating of the mother liquid and achieve rapid crystallization, an embodiment of the present invention provides a crystallization device.

[0005] The embodiment of the utility model provides a crystallization device, comprising a mother liquor tank, an oscillating temperature crystallization tube and a crystallization tank;

[0006] The oscillating temperature crystallizer includes multiple low-temperature crystallizers and multiple high-temperature melting crystallizers, with the multiple low-temperature crystallizers and multiple high-temperature melting crystallizers being connected alternately, and the first and last ones being the low-temperature crystallizers. The mother liquor tank is connected to the first low-temperature crystallizer in the oscillating temperature crystallizer, and the crystallization tank is connected to the last low-temperature crystallizer in the oscillating temperature crystallizer.

[0007] In one embodiment, the crystallization device further includes a low-temperature medium layer covering the low-temperature crystallization tube.

[0008] In one embodiment, the crystallization device further includes a high-temperature medium layer covering the high-temperature crystal dissolving tube.

[0009] In one embodiment, a first temperature measuring device is provided in the low-temperature crystallization tube.

[0010] In one embodiment, a second temperature measuring device is provided in the high-temperature crystal dissolving tube.

[0011] In one embodiment, a first valve is provided on the connecting pipe between the mother liquor tank and the low-temperature crystallization tube.

[0012] In one embodiment, a second valve is provided on the connecting pipe between the low-temperature crystallization tube and the adjacent high-temperature crystal dissolution tube.

[0013] In one embodiment, a third valve is provided on the connecting pipe between the crystallization tank and the low-temperature crystallization tube.

[0014] In one embodiment, a first piston is provided in the low-temperature crystallization tube, and a second piston is provided in the high-temperature crystal dissolution tube.

[0015] In one embodiment, in the oscillating temperature crystallization tube, the low-temperature crystallization tube and the high-temperature crystal dissolution tube are arranged in parallel, and the first piston and the second piston are respectively arranged at two ends along the extension direction of the low-temperature crystallization tube.

[0016] In the crystallization device provided by the embodiment of the present invention, the mother liquor to be crystallized is finally collected into the crystallization tank from the mother liquor tank through the oscillating temperature crystallization tubes which are alternately arranged as low-temperature crystallization tubes and high-temperature crystal dissolving tubes. The mother liquor to be crystallized can be continuously cooled and heated in sequence by the above device, and the crystallized material can be quickly obtained by using the oscillating temperature crystallization. Attached Figure Description

[0017] In order to more clearly illustrate the specific implementation methods of the utility model or the technical solutions in the prior art, the drawings required for use in the specific implementation methods or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are some implementation methods of the utility model. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.

[0018] Figure 1 This is an implementation of the crystallization device provided by the utility model.

[0019] Description of reference numerals:

[0020] 10: Crystallization device; 100: Mother liquor tank; 101: First valve; 200: Oscillating temperature crystallization tube; 201: Low-temperature crystallization tube; 202: High-temperature dissolving crystal tube; 203: Low-temperature medium layer; 2031: Low-temperature medium inflow channel; 2032: Low-temperature medium outflow channel; 204: High-temperature medium layer; 2041: High-temperature medium inflow channel; 2042: High-temperature medium outflow channel; 205: First piston; 206: Second piston; 207: Second valve; 208: Third valve; 300: Crystallization tank. DETAILED DESCRIPTION

[0021] To facilitate understanding of the present invention, a more comprehensive description of the present invention will be provided below with reference to the accompanying drawings. The drawings illustrate preferred embodiments of the present invention. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to facilitate a more thorough and comprehensive understanding of the disclosure of the present invention.

[0022] In the description of the present invention, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inside", "outside", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like to indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation to the present invention.

[0023] Furthermore, the terms "first" and "second" are used for descriptive purposes only and should not be construed as indicating or implying relative importance or implicitly specifying the number of the technical features being referred to. Thus, a feature specified as "first" or "second" may explicitly or implicitly include at least one such feature. In the description of this utility model, "plurality" means at least two, such as two, three, etc., unless otherwise specifically defined.

[0024] In this utility model, unless otherwise specified or limited, the terms "installed," "connected," "connect," "fixed," etc. should be understood in a broad sense. For example, they can refer to fixed connection, detachable connection, or integration; mechanical connection, electrical connection; direct connection, or indirect connection through an intermediate medium; internal communication between two components, or interaction between two components, unless otherwise specified. Those skilled in the art will understand the specific meanings of the above terms in this utility model based on specific circumstances.

[0025] In the present invention, unless otherwise expressly specified or limited, when a first feature is "above" or "below" a second feature, it may mean that the first and second features are in direct contact, or the first and second features are in indirect contact through an intermediary. Furthermore, when a first feature is "above," "above," or "above" a second feature, it may mean that the first feature is directly above or diagonally above the second feature, or simply means that the first feature is at a higher level than the second feature. When a first feature is "below," "below," or "below" a second feature, it may mean that the first feature is directly below or diagonally below the second feature, or simply means that the first feature is at a lower level than the second feature.

[0026] It should be noted that when an element is referred to as being "fixed to" or "set on" another element, it may be directly on the other element or there may also be an element centered. When an element is considered to be "connected to" another element, it may be directly connected to the other element or there may be an element centered at the same time. The terms "vertical", "horizontal", "up", "down", "left", "right" and similar expressions used herein are for illustrative purposes only and are not intended to be the only implementation method. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which the present invention pertains. The terms used herein in the specification of the present invention are for the purpose of describing specific embodiments only and are not intended to limit the present invention. The term "and / or" used herein includes any and all combinations of one or more of the relevant listed items.

[0027] This utility model provides a crystallization device 10, including a mother liquor tank 100, a oscillating temperature crystallization tube 200, and a crystallization tank 300.

[0028] The oscillating temperature crystallization tubes 200 include multiple low-temperature crystallization tubes 201 and multiple high-temperature crystal dissolving tubes 202. The multiple low-temperature crystallization tubes 201 are alternately connected to the multiple high-temperature crystal dissolving tubes 202, with both low-temperature crystallization tubes 201 at the beginning and end. It is understood that the number of low-temperature crystallization tubes 201 exceeds the number of high-temperature crystal dissolving tubes 202 by one. The mother liquor tank 100 is connected to the first low-temperature crystallization tube 201 in the oscillating temperature crystallization tubes 200. The crystallization tank 300 is connected to the last low-temperature crystallization tube 201 in the oscillating temperature crystallization tubes 200.

[0029] The temperature difference between the high-temperature crystallization tube and the low-temperature crystallization tube is the oscillation temperature, which is generally designed based on the solvent composition of the mother liquor. The temperature difference ranges from 5℃ to 100℃. For common organic molecules, when the solvent is mainly a low-boiling-point organic solvent, such as one or more of ethyl acetate, dichloromethane, acetone, tetrahydrofuran, methanol, ethanol, and n-hexane, the temperature difference can be limited to 10℃~30℃. For complexes or ionic crystals containing metals, the solvent is generally one or more high-boiling-point solvents such as N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N-methylpyrrolidone (NMP), ethylene glycol methyl ether (2-ME), and γ-butyrolactone (GBL), and the temperature difference can be limited to 10℃~50℃.

[0030] Understandably, adjacent low-temperature crystallizers 201 and high-temperature melting crystallizers 202 in the oscillating temperature crystallizer 200 are arranged in parallel. Preferably, the mother liquor tank 100 has two connection points with the first low-temperature crystallizer 201 in the oscillating temperature crystallizer 200, which are the two ends in the extension direction of the low-temperature crystallizer 201; adjacent low-temperature crystallizers 201 and high-temperature melting crystallizers 202 have two connection points, which are the two ends in the extension direction of the low-temperature crystallizer 201; and the crystallizer tank 300 has two connection points with the last low-temperature crystallizer 201 in the oscillating temperature crystallizer 200, which are the two ends in the extension direction of the low-temperature crystallizer 201.

[0031] In a specific example, the oscillating temperature crystallization tube 200 further includes a low-temperature medium layer 203 covering the low-temperature crystallization tube 201. Furthermore, a low-temperature medium inflow channel 2031 and a low-temperature medium outflow channel 2032 are provided on the surface of the low-temperature medium layer 203.

[0032] Understandably, adjacent low-temperature crystallizers 201 and high-temperature melting crystallizers 202 in the oscillating temperature crystallizer 200 are arranged in parallel and horizontally. The low-temperature medium enters the low-temperature medium layer 203 through the low-temperature medium inflow channel 2031 and exits the low-temperature medium layer 203 through the low-temperature medium outflow channel 2032. Further, the low-temperature medium inflow channel 2031 is located at the bottom of the low-temperature crystallizer 201 in the vertical direction, and the low-temperature medium outflow channel 2032 is located at the top of the low-temperature crystallizer 201 in the vertical direction. Even further, the low-temperature medium inflow channel 2031 is located at the bottom of one side of the low-temperature crystallizer 201 in the extension direction, and the low-temperature medium outflow channel 2032 is located at the top of the other side of the low-temperature crystallizer 201 in the extension direction, so that the low-temperature medium can fully cover the low-temperature crystallizer 201 before flowing out, allowing the low-temperature crystallizer 201 to reach the required temperature.

[0033] In a specific example, a first temperature measuring device is provided in the low-temperature crystallization tube 201. The first temperature measuring device is a thermocouple temperature measuring device, and the flow rate and temperature of the low-temperature medium are adjusted as needed based on the temperature data obtained by the first temperature measuring device.

[0034] In a specific example, the oscillating temperature crystallization tube 200 further includes a high temperature medium layer 204 covering the high temperature crystal dissolving tube 202. Furthermore, a high temperature medium inflow channel 2041 and a high temperature medium outflow channel 2042 are provided on the surface of the high temperature medium layer 204.

[0035] It is understood that the adjacent low-temperature crystallization tube 201 and high-temperature crystal dissolving tube 202 in the oscillating temperature crystallization tube 200 are arranged parallel and horizontally. The high-temperature medium enters the high-temperature medium layer 204 through the high-temperature medium inflow channel 2041 and then flows out of the high-temperature medium layer 204 through the high-temperature medium outflow channel 2042. Furthermore, the high-temperature medium inflow channel 2041 is arranged at the bottom of the high-temperature crystal dissolving tube 202 in the vertical direction, and the high-temperature medium outflow channel 2042 is arranged at the top of the high-temperature crystal dissolving tube 202 in the vertical direction. Furthermore, the high-temperature medium inflow channel 2041 is arranged at the bottom of one side of the high-temperature crystal dissolving tube 202 in the direction of extension, and the high-temperature medium outflow channel 2042 is arranged at the top of the other side of the high-temperature crystal dissolving tube 202 in the direction of extension. This ensures that the high-temperature medium fully covers the high-temperature crystal dissolving tube 202 before flowing out, allowing the high-temperature crystal dissolving tube 202 to reach the desired temperature.

[0036] In a specific example, a second temperature measuring device is provided in the high-temperature crystal dissolving tube 202. The second temperature measuring device is a thermocouple temperature measuring device, and the flow rate and temperature of the high-temperature medium are adjusted as needed based on the temperature data obtained by the second temperature measuring device.

[0037] Understandably, the solubility-temperature curve of a substance follows a logarithmic function, meaning that a high-temperature saturated solution experiences a more pronounced solubility change during the initial temperature ramp. Therefore, as the mother liquor from the high-temperature crystal dissolution tube 202 flows into the initial low-temperature crystallization tube 201, the cooling process must be slow and precise. Therefore, the temperatures of the low-temperature crystallization tube 201 and the high-temperature crystal dissolution tube 202 in the present invention can also be set in a gradient to achieve optimal crystallization conditions.

[0038] In a specific example, a first valve 101 is provided on the connecting pipe between the mother liquor tank 100 and the low-temperature crystallization tube 201 .

[0039] In a specific example, a second valve 207 is provided on the connecting pipe between the low-temperature crystallization tube 201 and the adjacent high-temperature crystal dissolution tube 202 .

[0040] In a specific example, a third valve 208 is provided on the connecting pipe between the crystallization tank 300 and the last low-temperature crystallization tube 201 in the oscillating temperature crystallization tube 200 .

[0041] Preferably, the first valve 101, the second valve 207, and the third valve 208 are all one-way valves. Each of these one-way valves can be connected to the atmosphere, allowing selected pipelines to be vented independently, similar to a magnetically controlled three-way valve.

[0042] In a specific example, a first piston 205 is provided in the low-temperature crystallization tube 201 , and a second piston 206 is provided in the high-temperature crystal dissolution tube 202 .

[0043] It can be understood that the first piston 205 and the second piston 206 are connecting rod-less pistons.

[0044] In a specific example, the low-temperature crystallizer 201 and the high-temperature melting crystallizer 202 are arranged in parallel in the oscillating temperature crystallizer 200, and the first piston 205 and the second piston 206 are respectively arranged at both ends along the extension direction of the low-temperature crystallizer 201.

[0045] As the first piston 205 and the second piston 206 reciprocate, they move towards each other. With the help of the check valve, the mother liquor can only be drawn in from the previous tank / pipeline and injected into the next pipe / tank.

[0046] Specifically, according to Figure 1 In the crystallization device 10 shown, the mother liquor flows in from the connection between the mother liquor tank 100 and the first low-temperature crystallization tube 201 in the oscillating temperature crystallization tube 200 near the first piston 205, and the first piston 205 and the second piston 206 arranged opposite to each other move simultaneously, so that the mother liquor is drawn from the mother liquor tank 100 into the first low-temperature crystallization tube 201, and then drawn from the first low-temperature crystallization tube 201 by the second piston 206 into the high-temperature crystal dissolving tube 202 connected thereto, and then drawn into the next low-temperature crystallization tube 201, and this is repeated until it is finally drawn into the last low-temperature crystallization tube 201 in the oscillating temperature crystallization tube 200, and finally drawn into the crystallization tank 300.

[0047] It can be understood that in order to obtain the expected quality of the crystallization product in the crystallization device 10 provided by the present invention, the flow rate of the mother liquor, the speed of the piston movement, the length of time the mother liquor stays in each pipe of the oscillating temperature crystallization tube 200, the temperature of the low-temperature crystallization tube 201 and the high-temperature crystal dissolving tube 202 in the oscillating temperature crystallization tube 200, and the number of the low-temperature crystallization tube 201 and the high-temperature crystal dissolving tube 202 can be adjusted as needed. All of these can be monitored and controlled by the integrated system, and can also be set according to the crystallization process of different substances and the expected quality of the crystallization product.

[0048] It should also be noted that the crystallization device 10 can be placed horizontally or vertically as needed. Figure 1 A way of placing.

[0049] The crystallization apparatus 10 provided by the present invention provides a mother liquor to be crystallized. The mother liquor to be crystallized flows from the mother liquor tank 100 through the alternating low-temperature crystallization tubes 201 and high-temperature crystal dissolving tubes 202, which are oscillating temperature crystallization tubes 200, and finally converges into the crystallization tank 300. The mother liquor to be crystallized can be continuously cooled and heated sequentially by the apparatus, and the oscillating temperature crystallization can rapidly obtain a crystalline material. The apparatus can be used for large-scale industrial production.

[0050] 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. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0051] The technical features of the above embodiments can be combined arbitrarily. To make the description concise, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0052] The above-described embodiments are merely illustrative of several implementations of this utility model, designed to facilitate a detailed understanding of the technical solution of this utility model, but should not be construed as limiting the scope of patent protection. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of this utility model, and these all fall within the scope of protection of this utility model. It should be understood that technical solutions obtained by those skilled in the art based on the technical solutions provided by this utility model through logical analysis, reasoning, or limited experimentation are all within the scope of protection of the appended claims. Therefore, the scope of protection of this utility model patent should be determined by the content of the appended claims, and the specification can be used to interpret the content of the claims.

Claims

1. A crystallization device, characterized in that: It includes a mother liquor tank, an oscillating temperature crystallization tube and a crystallization tank; The oscillating temperature crystallization tube includes a plurality of low-temperature crystallization tubes and a plurality of high-temperature crystal dissolving tubes, wherein the plurality of low-temperature crystallization tubes are alternately connected with the plurality of high-temperature crystal dissolving tubes and the head and tail are both the low-temperature crystallization tubes, wherein the mother liquor tank is connected to the first low-temperature crystallization tube among the oscillating temperature crystallization tubes, and the crystallization tank is connected to the last low-temperature crystallization tube among the oscillating temperature crystallization tubes.

2. The crystallization device according to claim 1, characterized in that The crystallization device also includes a low-temperature medium layer covering the low-temperature crystallization tube.

3. The crystallization device according to claim 1, characterized in that The crystallization device also includes a high-temperature medium layer covering the high-temperature crystal dissolving tube.

4. The crystallization device according to claim 1, characterized in that A first temperature measuring device is arranged in the low-temperature crystallization tube.

5. The crystallization device according to claim 1, characterized in that A second temperature measuring device is arranged in the high-temperature crystal dissolving tube.

6. The crystallization device according to claim 1, characterized in that A first valve is provided on the connecting pipeline between the mother liquid tank and the low-temperature crystallization tube.

7. The crystallization device according to claim 1, characterized in that A second valve is provided on the connecting pipe between the low-temperature crystallization tube and the adjacent high-temperature crystal dissolving tube.

8. The crystallization device according to claim 1, characterized in that A third valve is provided on the connecting pipeline between the crystallization tank and the low-temperature crystallization tube.

9. The crystallization device according to any one of claims 1 to 8, characterized in that: A first piston is arranged in the low-temperature crystallization tube, and a second piston is arranged in the high-temperature crystal dissolving tube.

10. The crystallization device according to claim 9, characterized in that In the oscillating temperature crystallization tube, the low-temperature crystallization tube is arranged in parallel with the high-temperature crystal dissolving tube, and the first piston and the second piston are respectively arranged at two ends along the extension direction of the low-temperature crystallization tube.

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