A continuous crystallization polymorph control system

Abstract

The utility model relates to a kind of continuous crystallization crystal form control systems, comprising: liquid supply module, including mother liquor kettle, liquid feed pipe connected in the inlet end of mother liquor kettle and liquid discharge pipe connected in the outlet end of mother liquor kettle;Hot melting module, including hot melting kettle, the hot melting kettle is equipped with two feeding ends and a discharge end, one feeding end is used for fixed material feeding, another feeding end is connected to the liquid discharge pipe, and the discharge end is connected with dissolved material discharge pipe;Crystallization module, including refrigerant heat exchange component and heat medium heat exchange component, the refrigerant heat exchange component includes the refrigerant heat exchanger connected in dissolved material discharge pipe, and the heat medium heat exchange component includes the heat medium heat exchanger connected in refrigerant heat exchanger;Filter module, including the doctor centrifuge for material filtration, and its inlet end is connected to heat medium heat exchange component.The utility model can realize continuous crystallization, stable crystallization, avoid the crystal form change caused by product secondary crystallization, and can reduce raw material cost.

Description

Technical Field

[0001] This utility model relates to the field of crystallization form control technology, specifically a continuous crystallization form control system. Background Technology

[0002] In the OLED field, sublimation is an important process, primarily used for the purification of OLED materials and device fabrication. During sublimation, the product is typically placed in a sublimation tube or similar container, and a vacuum pump is used to evacuate the chamber to a high vacuum state. The product is then sublimated by heating. During sublimation, inconsistencies in the product's bulk density can lead to significant fluctuations in the sublimation rate, sublimation uniformity, and material utilization. These variations in bulk density are mainly due to unstable crystal form control during the product manufacturing process.

[0003] In chemical production, crystallization is the process by which a solute transforms from a liquid phase into a solid crystal. Its core is the formation of a periodic crystal structure through the ordered arrangement of molecules, atoms, or ions. In the production of organic chemicals, products are purified into solids through crystallization. However, due to the numerous controllable factors in the crystallization process, complete consistency cannot be guaranteed, leading to inconsistent crystal forms and varying bulk densities in the produced products, which in turn affects the sublimation efficiency. Utility Model Content

[0004] The purpose of this invention is to provide a continuous crystallization crystal form control system that can achieve stable crystal precipitation during the crystallization process and ensure the stability of the product crystal form.

[0005] To achieve the above objectives, this utility model provides the following technical solution: a continuous crystallization crystal form control system, comprising a liquid supply module, a hot melting module, a crystallization module, and a filtration module. The liquid supply module includes a mother liquor tank, a liquid feed pipe connected to the inlet end of the mother liquor tank, and a liquid discharge pipe connected to the outlet end of the mother liquor tank. The hot melting module includes a hot melting tank, which has two feeding ends and one discharge end. One feeding end is used for fixed material feeding, and the other feeding end is connected to the liquid discharge pipe for liquid material feeding. The discharge end is connected to a dissolved substance discharge pipe. The crystallization module includes a refrigerant heat exchange component and a heat exchange component. The refrigerant heat exchange component includes a refrigerant heat exchanger connected to the dissolved substance discharge pipe, and the heat exchange component includes a heat exchanger connected to the refrigerant heat exchanger. The filtration module includes a scraper centrifuge for material filtration, the inlet end of which is connected to the heat exchange component.

[0006] In a preferred embodiment, the dissolved material outlet pipe is also connected to a flow meter, which is used to monitor flow fluctuations during the continuous crystallization process to ensure the stability and continuity of the continuous crystallization process.

[0007] In a preferred embodiment, the refrigerant heat exchanger is connected to a refrigerant temperature control system for refrigerant supply and regulation, and / or the heat exchanger is connected to a heat medium temperature control system for heat medium supply and regulation. The temperature control system allows adjustment of the refrigerant / heat medium temperature according to actual needs, thereby controlling the crystallization rate.

[0008] In a preferred embodiment, the number of refrigerant heat exchange components is set to multiple groups to achieve staged cooling.

[0009] In a preferred embodiment, the discharge end of the scraper centrifuge is connected to the mother liquor tank to achieve mother liquor circulation.

[0010] In a preferred embodiment, the liquid supply module further includes a weighing module connected to the mother liquor tank.

[0011] In a preferred embodiment, the number of hot melt kettles is set to two, and the two hot melt kettles are distributed in parallel and operate alternately to achieve uninterrupted connection and crystallization.

[0012] Compared with the prior art, the beneficial effects of this utility model are:

[0013] The continuous crystallization crystal form control system provided by this utility model can realize continuous crystallization. Through the cooperation of the refrigerant heat exchange component and the heat exchange component in the crystallization module, the crystal form change caused by secondary crystallization of the product can be avoided, ensuring the stability of the product crystal form. Moreover, through the cooperation of the mother liquor circulation structure and the heat exchanger, not only can the mother liquor be recycled and the cost reduced, but the impact on the stability of crystal nucleus formation caused by mother liquor circulation and impurity enrichment can also be reduced. Attached Figure Description

[0014] Figure 1 A schematic diagram of the structure of the continuous crystallization crystal form control system provided in the embodiment of this utility model.

[0015] The meanings of the labels in the diagram are as follows:

[0016] 1. Mother liquor tank; 2. Liquid inlet pipe; 3. Liquid outlet pipe; 4. Automatic bottom valve; 5. Magnetic pump; 6. Weighing module; 7. Hot melt tank; 8. Vacuum feeder; 9. Self-controlled bottom valve; 10. Flow meter; 11. Metering pump; 12. Refrigerant heat exchanger; 13. Refrigerant constant temperature system; 14. Pipe insulation components; 15. Heat exchanger; 16. Heat exchanger constant temperature system; 17. Scraper centrifuge; 18. Diaphragm pump; 19. Dissolved matter outlet pipe; 20. First outlet pipe; 21. Second outlet pipe; 22. Third outlet pipe. Detailed Implementation

[0017] 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. Based on the embodiments of the present utility model, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the protection scope of the present utility model.

[0018] In the description of this utility model, it should be understood that the terms "center", "longitudinal", "lateral", "length", "width", "thickness", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", and "outer" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this utility model and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this utility model.

[0019] See Figure 1 This embodiment discloses a continuous crystallization crystal form control system, including a liquid supply module, a hot melting module, a crystallization module, and a filtration module.

[0020] The liquid supply module includes a mother liquor tank 1, a liquid feed pipe 2 connected to the inlet end of the mother liquor tank 1, and a liquid discharge pipe 3 connected to the outlet end of the mother liquor tank 1. The liquid discharge pipe 3 is connected to an automatic bottom valve 4 and a magnetic pump 5.

[0021] The hot melt module includes a hot melt kettle 7, which has two feeding ends and one discharging end. The first feeding end is connected to a vacuum feeder 8 for fixing the material feeding. The second feeding end is connected to the aforementioned liquid discharge pipe 3 for feeding liquid materials. The liquid and solid materials are heated and dissolved in the hot melt kettle 7. The dissolved organic solution is discharged through the dissolved material discharge pipe 19 connected to the discharging end of the hot melt kettle 7. The dissolved material discharge pipe 19 is connected to a self-controlled bottom valve 9, a flow meter 10, and a metering pump 11. The flow meter 10 is used to monitor the flow fluctuation during the continuous crystallization process to ensure the stability and continuity of the continuous crystallization process.

[0022] The crystallization module includes refrigerant heat exchange components and heat exchange components that are interconnected.

[0023] Specifically, the refrigerant heat exchange assembly includes a refrigerant heat exchanger 12, which has an inlet end and an outlet end. The inlet end is connected to the dissolved substance outlet pipe 19, and the outlet end is connected to the heat exchange assembly via a first outlet pipe 20. The dissolved substance enters the refrigerant heat exchanger 12 for crystallization. The refrigerant heat exchanger 12 is connected to a refrigerant temperature control system 13 for refrigerant supply and regulation. The refrigerant temperature control system 13 can adjust the refrigerant temperature according to actual needs to regulate the crystallization rate. The first outlet pipe 20 is also fitted with a pipe insulation component 14. By precisely controlling the flow rate of the dissolved substance through the refrigerant heat exchanger 12 via a flow meter 10 and by precisely controlling the refrigerant temperature, product performance stability and uniform crystallization can be promoted.

[0024] Ideally, depending on the product characteristics, the number of refrigerant heat exchange components can be increased and staged cooling can be implemented. This setting is more conducive to the control of the crystal form precipitated by the product, making the system applicable to a wider range of product types.

[0025] The structures of the heat exchanger assembly and the refrigerant heat exchanger assembly are largely the same, including a heat exchanger 15. The heat exchanger 15 also has an inlet and an outlet. Its inlet is connected to the first outlet pipe 20 of the refrigerant heat exchanger assembly, and its outlet is connected to the filter module via a second outlet pipe 21. The heat exchanger 15 is connected to a heat exchanger temperature control system 16 for heat supply and regulation. The heat exchanger temperature control system 16 can adjust the heat exchanger temperature according to actual needs. In this embodiment, both the refrigerant temperature control system 13 and the heat exchanger temperature control system 16 adopt existing technologies. The second outlet pipe 21 is also fitted with a pipe insulation component 14.

[0026] This embodiment, by adding a constant-temperature heat transfer medium structure after the refrigerant structure, can avoid the crystal form change caused by secondary crystallization of the product and ensure the stability of the product's crystal form.

[0027] The filtration module is used for material filtration. Its inlet is connected to the heat exchanger assembly at the front end, and its outlet is connected to the mother liquor tank 1 of the liquid supply module, thereby circulating the mother liquor. Specifically, the filtration module includes a scraper centrifuge 17 for material filtration. Its inlet is connected to the second outlet pipe 21, and its outlet is connected to the mother liquor tank 1 via a third outlet pipe 22. The third outlet pipe 22 is connected to a diaphragm pump 18. Furthermore, the material exiting the heat exchanger 15 is transported to the scraper centrifuge 17 for filtration. The solids filtered from the scraper centrifuge 17 are collected separately, and the filtered mother liquor is fed back into the mother liquor tank 1 for recycling via the diaphragm pump 18, thereby reducing raw material costs.

[0028] Preferably, the liquid supply module also includes a weighing module 6 connected to the mother liquor tank 1. The weighing module 6 can precisely control the weight of the liquid raw material in the mother liquor tank 1, thereby controlling the input amount of the liquid raw material in the hot melt reactor 7 and keeping it constant. In this embodiment, the liquid feed pipe 2 connected to the inlet end of the mother liquor tank 1 can serve as a replenishment pipe. Based on the weight of the mother liquor in the mother liquor tank 1 measured by the weighing module 6, liquid is replenished in real time through the liquid feed pipe 2, reducing batch variations.

[0029] It should be noted that although mother liquor circulation can reduce costs during continuous crystallization, it can also lead to the enrichment of impurities. These impurities can affect the crystal nucleus formation temperature and disrupt its stability. In this embodiment, by precisely controlling the temperature of the heat exchanger 15 in the crystallization module, the interaction between impurities and solute can be disrupted, and microcrystals generated by composition fluctuations can be dissolved. This counteracts the interference of composition fluctuations on the crystal form and further promotes the stability of the crystal form.

[0030] Preferably, in the hot melt module, the number of hot melt kettles 7 is set to two, and the two hot melt kettles 7 are distributed in parallel. When the production batch is large, the two hot melt kettles 7 work alternately to achieve uninterrupted connection and crystallization.

[0031] In practical applications, solid materials are automatically fed into the hot melt kettle via vacuum feeder 8, while liquid materials are weighed by mother liquor kettle 1 and weighing module 6 before being fed into hot melt kettle 7. After the solid and liquid dissolve, automatic bottom valve 4 and metering pump 11 are opened, and the dissolved solution is uniformly introduced into refrigerant heat exchanger 12 via flow meter 10 for crystallization. Then, it is heated by heat medium heat exchanger 15 to prevent secondary precipitation of the product. After filtration by scraper centrifuge 17, the solid material is collected separately, and the filtered mother liquor is returned to mother liquor kettle 1. Liquid material is added according to the weight of the mother liquor. After hot melt kettle 7 is empty, the second feeding and crystallization process is carried out to achieve continuous crystallization. Through the automated control system, stable continuous crystallization can be achieved, improving production efficiency and reducing production costs.

[0032] It is understood that the above-mentioned actions in this embodiment are all controlled by a control module. The control module may specifically include a controller that can control other modules according to a predetermined program, so that each module can start, stop or perform other actions according to a preset process. The control method of the controller can be implemented by simple programming by those skilled in the art, which is common knowledge in the field. Therefore, this embodiment will not explain the specific control method in detail.

[0033] The foregoing has shown and described the basic principles, main features, and advantages of this utility model. Those skilled in the art should understand that this utility model is not limited to the above embodiments. The embodiments and descriptions in the specification are merely preferred examples and are not intended to limit the utility model. Various changes and modifications can be made to this utility model without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claimed utility model. The scope of protection of this utility model is defined by the appended claims and their equivalents.

Claims

1. A continuous crystallization crystal form control system, characterized in that, include: The liquid supply module includes a mother liquor tank (1), a liquid feed pipe (2) connected to the inlet end of the mother liquor tank (1), and a liquid discharge pipe (3) connected to the outlet end of the mother liquor tank (1); The hot melt module includes a hot melt kettle (7), which has two feeding ends and one discharging end. One feeding end is used to fix the material feeding, and the other feeding end is connected to the liquid discharging pipe (3) for feeding liquid materials. The discharging end is connected to the dissolved material discharging pipe (19). The crystallization module includes a refrigerant heat exchange component and a heat exchange component. The refrigerant heat exchange component includes a refrigerant heat exchanger (12) connected to the dissolved substance outlet pipe (19), and the heat exchange component includes a heat exchanger (15) connected to the refrigerant heat exchanger (12). The filtration module includes a scraper centrifuge (17) for material filtration, the feed end of which is connected to a heat exchanger assembly.

2. The continuous crystallization crystal form control system according to claim 1, characterized in that, The dissolved material outlet pipe (19) is also connected to a flow meter (10).

3. The continuous crystallization crystal form control system according to claim 1, characterized in that, The refrigerant heat exchanger (12) is connected to a refrigerant constant temperature system (13) for refrigerant supply and regulation, and / or the heat exchanger (15) is connected to a heat medium constant temperature system (16) for heat medium supply and regulation.

4. The continuous crystallization crystal form control system according to claim 1, characterized in that, The number of refrigerant heat exchange components is set to multiple groups to achieve staged cooling.

5. The continuous crystallization crystal form control system according to claim 1, characterized in that, The discharge end of the scraper centrifuge (17) is connected to the mother liquor tank (1).

6. The continuous crystallization crystal form control system according to claim 1, characterized in that, The liquid supply module also includes a weighing module (6) connected to the mother liquor tank (1).

7. The continuous crystallization crystal form control system according to claim 1, characterized in that, The number of the hot melt kettles (7) is set to two, and the two hot melt kettles (7) are distributed in parallel.

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