CN108992962B - Modularized sublimation purification system - Google Patents

Modularized sublimation purification system Download PDF

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Publication number
CN108992962B
CN108992962B CN201811160080.1A CN201811160080A CN108992962B CN 108992962 B CN108992962 B CN 108992962B CN 201811160080 A CN201811160080 A CN 201811160080A CN 108992962 B CN108992962 B CN 108992962B
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module
area
collecting
cavity
feeding
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CN108992962A (en
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马飞越
韦国丹
黄俊豪
杨琛
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Shenzhen Purui Material Technology Co ltd
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Shenzhen Purui Material Technology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D7/00Sublimation

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention provides a modularized sublimation purification system, which comprises a feeding module, a collecting module, a connecting module, a heating module, a vacuumizing device and a background control system, wherein the feeding module comprises at least one feeding area, the collecting module comprises at least one collecting area, the connecting module comprises at least one connecting area, and a vacuum valve is arranged in a cavity of the connecting area; the heating module comprises a plurality of groups of heating wires and is used for heating the device. According to the invention, the heating wires are arranged in the cavity wall, and then the starting and stopping of each group of heating wires are controlled by the background control system to realize active temperature adjustment; the feeding module and the collecting module can be separated independently by the valve, and the feeding area and the collecting area are convenient to replace; a feeding zone and a plurality of collecting zones are connected in series through a connecting module, and a fine temperature zone is arranged in each collecting zone so as to realize continuous sublimation and purification of raw materials; the plurality of feeding areas are connected with the plurality of collecting areas in series and parallel through the connecting module, and large-scale sublimation and purification can be realized.

Description

Modularized sublimation purification system
Technical Field
The invention relates to the technical field of sublimation purification of organic materials, in particular to a modularized sublimation purification system.
Background
Organic materials are widely used in the Organic electronics field using Organic semiconductors, such as Organic Light Emitting Diode (OLED), organic solar cell (Organic Solar Cell, O-SC), organic thin film Transistor (Organic Thin Film Transistor, O-TFT), organic FIELD EFFECT Transistor (O-FET), organic integrated circuit (Organic Integrated Circuit, O-IC), organic laser Diode (O-laser), etc., wherein the OLED materials are highly focused on due to their advantages of spontaneous optical activity, high contrast, high reaction rate, wide viewing angle, low power consumption, full color, simple manufacturing process, etc., especially in the display and illumination fields.
For OLED devices, the purity of the main substances of the OLED materials directly affects the performance and reliability of the devices, and the OLED materials are divided into two main types from the technical direction at present: small molecular organic materials and high molecular materials. From the current commercial products, most manufacturers use small molecule OLED organic materials. Sublimation purification is the most useful and common purification method of small molecular materials of organic semiconductors by setting a temperature gradient, and the principle of the method is mainly to set a temperature gradient, and separate main substances from impurities in a manner of setting a sublimation temperature higher than that of a target material in a sublimation zone and setting a sublimation temperature lower than that of the target material in a collection zone for purification. However, the organic material usually contains various impurities with similar sublimation temperatures, and generally, the sublimation and purification by once heating cannot meet the purity requirement, the main material needs to be sublimated for the second time or even more times, the whole process consumes a lot of time, or continuous sublimation temperature intervals are set for sublimating to reach enough purity, so that the material discharging and material taking can be performed after the whole sublimation and purification process is completely finished, the time consumption is still quite long, and therefore, how to sublimate, separate and purify with high efficiency to obtain high-purity small molecular organic materials is a problem to be solved urgently at present.
Moreover, as shown in fig. 1, the existing sublimation purification method is generally performed in a vacuum environment of a quartz glass tube 10, a ceramic fiber plate 12 with an electric resistance heating wire 11 arranged inside is used for heating the quartz glass tube 10 outside, different temperature areas divide the quartz glass tube 10 into a high-temperature sublimation area 13, a material deposition area 14 and an impurity deposition area 15, only when the raw materials to be purified in the quartz glass tube 10 are completely sublimated, the vacuum system is closed to scrape out target materials from the quartz glass tube 10, the feeding and collecting processes are long, the purification efficiency is low, large-scale purification is not realized, and the quartz glass tube 10 ensures a high-vacuum environment for sublimation purification, but the temperature is controlled by an external heating device, so that the temperature in the sublimation purification cavity cannot be accurately controlled, a large amount of materials are condensed in the field with low temperature, and the raw materials are wasted. In real life, in order to obtain various high-purity target materials, the existing sublimation purification device cannot adapt to target materials with different sublimation temperatures and application requirements of various purities.
Accordingly, the prior art is still in need of improvement and development.
Disclosure of Invention
The invention aims to provide a modularized sublimation purification system, which aims to solve the problems that the existing sublimation purification system cannot purify raw materials on a large scale, cannot meet the purification requirements of target materials with different sublimation temperatures, cannot efficiently obtain high-purity target materials and the like.
In order to solve the problems, the technical scheme of the invention is as follows:
the modularized sublimation purification system comprises a feeding module, a collecting module, a connecting module, a heating module, a vacuumizing device and a background control system, wherein the feeding module is connected with the collecting module through the connecting module, the heating module is connected with the feeding module, the collecting module and the connecting module, the vacuumizing device is connected with the collecting module in series, and the heating module is connected with the background control system;
The feeding module comprises at least one feeding area, and the feeding area is a cavity with one end open;
The collecting module comprises at least one collecting area, and the collecting area is a cavity with two open ends;
The connecting module comprises at least one connecting area, the connecting area is a cavity with two open ends, the feeding area and the collecting area are connected in series through the connecting area to form an integrated cavity, the connecting areas are fastened through vacuum flanges, and a vacuum valve is arranged in the cavity of the connecting area;
the heating module comprises a plurality of groups of heating wires, and the start and stop of each group of heating wires are mutually independent and are used for heating the feeding module, the collecting module and the connecting module;
The vacuumizing device is used for vacuumizing the integrated cavity;
The background control system controls the temperature of the feeding module, the collecting module and the connecting module by controlling the heating module.
The modularized organic material sublimation purification system is characterized in that the material of the feeding area cavity, the collection area cavity and the connection area cavity is aluminum alloy or stainless steel.
The modularized organic material sublimation purification system comprises a heating module, a background control system and a plurality of heating wires, wherein the heating module further comprises a plurality of temperature sensors, each group of heating wires corresponds to one temperature sensor, and the temperature sensors are used for sending temperature signals to the background control system.
And the modularized organic material sublimation purification system is characterized in that a group of heating wires and corresponding temperature sensors are arranged in the cavity wall of the feeding area.
The modularized organic material sublimation purification system is characterized in that a group of heating wires and corresponding temperature sensors thereof are arranged in the cavity wall of the collecting area; the inside condensation collection platform that is provided with of collecting area can take out, condensation collection platform inside sets up multiunit heater strip and corresponding temperature sensor.
The modularized organic material sublimation purification system is characterized in that the connecting area is divided into two parts by the vacuum valve, a group of mutually independent heating wires and corresponding temperature sensors are respectively arranged in the cavity walls of the connecting area at two sides of the vacuum valve, and a group of heating wires and corresponding temperature sensors are arranged in the vacuum valve.
The modular organic material sublimation purification system, wherein the connection zone can also be modified into a valveless cavity with at least three openings for connecting a plurality of feeding zones and collecting zones.
The modularized organic material sublimation purification system is characterized in that a feeding area is connected with a plurality of collecting areas in series, the series connection is connected through a plurality of connecting areas, and each collecting area is provided with different temperatures through a background control system to form a multi-stage purification cavity for multi-stage purification of organic materials.
The modularized organic material sublimation purification system comprises a plurality of multi-stage purification cavities, wherein the multi-stage purification cavities are connected in parallel through a plurality of valveless cavity connecting areas with at least three openings and are used for sublimating and purifying organic materials in a large scale.
The beneficial effects of the invention include: the invention provides a modularized sublimation purification system, which can realize active temperature adjustment by arranging a heating wire inside a cavity wall and controlling the heating wire by a background control system; the vacuum valve is arranged on the connecting module, when the valve is closed, the feeding module and the collecting module can be separated independently, the feeding area and the collecting area are convenient to replace, and time is saved; a feeding area and a plurality of collecting areas are connected in series through a connecting module, and a fine temperature interval is arranged in each collecting area, so that continuous sublimation and purification of raw materials can be realized to obtain high-purity target materials; the plurality of feeding areas are connected with the plurality of collecting areas in series and parallel through the connecting module, large-scale sublimation purification can be achieved, and due to the arrangement of the vacuum valve, the feeding areas are independent from the collecting areas, target materials can be quickly changed or collected and taken out, consumed time is reduced, and sublimation purification is achieved at high efficiency.
Drawings
Fig. 1 is a side sectional view showing the structure of a conventional purifying apparatus provided by the present invention.
Fig. 2 is a side cross-sectional view of a modular sublimation purification system provided by the invention.
Fig. 3 is a side cross-sectional view of another modular sublimation purification system provided by the invention.
Fig. 4 is a side cross-sectional view of yet another modular sublimation purification system provided by the present invention.
Fig. 5 is a side cross-sectional view of a feed zone provided by the present invention.
Fig. 6 is a schematic side cross-sectional view of a collection area provided by the present invention.
Fig. 7 is a side cross-sectional view of a collection area provided by the present invention.
Fig. 8 is a schematic side cross-sectional view of a connection zone provided by the present invention.
Fig. 9 is a side cross-sectional view of a connecting region of a shut-off valve according to the present invention.
Fig. 10 is a side cross-sectional view of a junction area of an open valve according to the present invention.
Fig. 11 is a side cross-sectional view of a three-port valveless cavity connection region provided by the present invention.
Fig. 12 is a side cross-sectional view of a four-port valveless cavity connection region provided by the present invention.
Reference numerals illustrate: 10. a quartz glass tube; 11. an electric heating wire; 12. ceramic fiber board; 13. a high temperature sublimation zone; 14. a material deposition zone; 15. an impurity deposition region; 21. a feed zone; 22. a connection region; 23. a collection zone; 31. a heating wire; 32. a temperature sensor; 41. a vacuum valve; 51. a condensing and collecting table; 401. an external transmission rod; 402 an internally threaded rod; 403 valve plate; 404. a seal ring; 405. a screw; 406 a securing means; 4. screw holes; 501. a raised platform; 502. a substrate; 503. and a support handle.
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein the same or similar reference numerals refer to the same or similar elements or elements having the same or similar functions throughout. The embodiments described below by referring to the drawings are exemplary only for explaining the present invention and are not to be construed as limiting the present invention.
In the description of the present invention, it should be understood that the terms "center," "longitudinal," "transverse," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate an orientation or positional relationship based on that shown in the drawings, merely for convenience of describing the present invention and simplifying the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention. In the description of the present invention, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically connected, electrically connected or can be communicated with each other; can be directly connected or indirectly connected through an intermediate medium, and can be communicated with the inside of two elements or the interaction relationship of the two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
In the present invention, unless expressly stated or limited otherwise, a first feature "above" or "below" a second feature may include both the first and second features being in direct contact, as well as the first and second features not being in direct contact but being in contact with each other through additional features therebetween. Moreover, a first feature being "above," "over" and "on" a second feature includes the first feature being directly above and obliquely above the second feature, or simply indicating that the first feature is higher in level than the second feature. The first feature being "under", "below" and "beneath" the second feature includes the first feature being directly under and obliquely below the second feature, or simply means that the first feature is less level than the second feature.
The following disclosure provides many different embodiments, or examples, for implementing different features of the invention. In order to simplify the present disclosure, components and arrangements of specific examples are described below. They are, of course, merely examples and are not intended to limit the invention. Furthermore, the present invention may repeat reference numerals and/or letters in the various examples, which are for the purpose of brevity and clarity, and which do not themselves indicate the relationship between the various embodiments and/or arrangements discussed. In addition, the present invention provides examples of various specific processes and materials, but one of ordinary skill in the art will recognize the application of other processes and/or the use of other materials.
Referring to fig. 2 to 10, in the embodiment shown in fig. 2, 3 and 4, the modularized organic material sublimation purification system provided by the invention comprises a feeding module, a collecting module, a connecting module, a heating module, a vacuumizing device and a background control system, wherein the feeding module and the collecting module are connected through the connecting module, the heating module is connected with the feeding module, the collecting module and the connecting module, the vacuumizing device is connected with the collecting module in series, and the heating module is connected with the background control system.
Further, the feeding module comprises at least one feeding area 21, as shown in fig. 5, the feeding area 21 is a cavity with one open end; the collecting module comprises at least one collecting area 23, as shown in fig. 6, the collecting area 23 is a cavity with two open ends; the connection module comprises at least one connection area 22, as shown in fig. 8, the connection area 22 is a cavity with two open ends, the feeding area 21 and the collecting area 23 are connected in series through the connection area 22 to form an integrated vacuum cavity, in practical application, the material constituting the feeding area 21 cavity, the collecting area 23 cavity and the connection area 22 cavity is aluminum alloy or stainless steel, in practical application, the sublimation temperature of the organic material can not exceed 400 ℃, the material of the cavity is aluminum alloy, and when the sublimation temperature of the organic material to be purified needs to be set at a temperature higher than 500 ℃, the preferred material of the cavity is stainless steel. As shown in fig. 2,3 and 4, the joints are secured by vacuum flanges (not shown).
In practical application, the heating module includes a plurality of groups of heating wires 31, as shown in fig. 2 and 3, the start and stop of each group of heating wires 31 are independent, and further, the heating module further includes a temperature sensor 32 corresponding to each group of heating wires 31, where the heating wires 31 are used for heating the feeding module, the collecting module and the connecting module; the temperature sensors 32 are used for sending temperature signals to a background control system, and the background control system controls each group of heating wires 31 through the temperature signals reacted by each temperature sensor 32 to control the temperature of each feeding zone 21, each collecting zone 23 and each connecting zone 22.
In practical application, a group of heating wires and corresponding temperature sensors are arranged in the wall of the cavity of the feeding zone 21. As shown in fig. 7, a group of heating wires 31 and corresponding temperature sensors 32 are arranged in the cavity wall of the collecting area 23; the bottom of the collecting area 23 is provided with a condensation collecting table 51 which can be taken out downwards and an opening matched with the condensation collecting table, the upper part of the condensation collecting table 51 is provided with a raised platform 501, the fitting area of the opening and the raised platform 501 is the same as the upper surface area of the raised platform 501, the middle part of the condensation collecting table 51 is provided with a round or square substrate 502, in the embodiment shown in fig. 6 or 7, the area of the raised platform 501 is smaller than the area of the substrate 502, and the raised platform 501 is positioned above the substrate 502; the base plate 502 closely fixes the raised platform 501 and the opening by means of the locking screw 405 and the screw hole 4 corresponding to the locking screw 405. In practical application, the outer edge of the substrate 502 is provided with a plurality of screw holes 4, the outer edge of the opening below the cavity is provided with screw holes 4 matched with the screw holes 4 of the substrate 502, and the substrate 502 and the opening below the cavity are locked by means of the locking screw 405, so that the raised platform 501 and the opening below the cavity are tightly sealed and fixed. Further, a sealing ring 404 is disposed around the lower end of the raised platform 501 to ensure a vacuum environment when the organic material sublimates, the lower part of the condensation collection platform 51 is a support handle 503, which can be a cylinder, so that the condensation collection platform 51 can be conveniently taken out, multiple groups of heating wires 31 and corresponding temperature sensors 32 are disposed inside the raised platform 501 at the upper part of the condensation collection platform 51, the raised platform 501 is disposed from edge to center into two temperature areas through a background control system, the two temperature areas are respectively provided with a group of heating wires 31 and corresponding temperature sensors 32, the temperature of the edge temperature area of the raised platform 501 is higher than the lowest sublimation temperature of the pure product of the target material, the temperature of the center temperature area is far lower than the lowest sublimation temperature of the pure product of the target material, each group of heating wires 31 and corresponding temperature sensors 32 thereof operate independently by virtue of a background control system, the temperature distribution condition of the surface of the condensation collection platform 51 can be controlled, the target material is prevented from being deposited in the edge area difficult to collect, and the temperature of the center temperature area of the raised platform 501 of the condensation collection platform 51 is far lower than the temperature of other parts of the cavity inner wall of the collection area 23, the temperature difference is sharp, so that the target material can be conveniently collected in the concentrated temperature area. In practical application, the upper part, the middle part and the lower part of the condensation collection platform 51 are integrally formed.
Further, as shown in fig. 8, a vacuum valve 41 is disposed in the cavity of the connection region 22, the vacuum valve 41 divides the connection region 22 into two parts, and two groups of mutually independent heating wires and corresponding temperature sensors are disposed in the cavity walls of the connection region 22 at two sides of the vacuum valve 41. The temperature of each side of the vacuum valve 41 is the same as the temperature of the area connected with the vacuum valve 41, as shown in fig. 2, the temperature of the left side of the vacuum valve 41 is kept consistent with the temperature of the feeding area 21, the temperature of the right side of the vacuum valve 41 is kept consistent with the temperature of the collecting area 23, the vacuum valve 41 of the connecting module is opened in the sublimation process of organic materials, the vacuum valve 41 is closed after the materials in the feeding area are used, the feeding area is cooled by a background control system, a group of heating wires and corresponding temperature sensors are arranged in the vacuum valve 41, and the high temperature of the side of the vacuum valve 41 facing the collecting area 23 is kept in the cooling process so as to avoid the sudden condensation of target products on the vacuum valve 41. In practical application, as shown in fig. 9, the external motor drives the external transmission rod 401 to rotate clockwise to drive the internal threaded rod 402 to rotate along with the external transmission rod 401, then the valve plate 403 moves downwards under the rotation drive of the internal threaded rod, the vacuum valve is closed, the external transmission rod 401 is fixed on the connection area 22 by the fixing device 406 locked by the screw 405, and the connection parts are all provided with the sealing rings 404 to ensure the vacuum environment when the organic material sublimates; as shown in fig. 10, the external motor drives the external transmission rod 401 to rotate anticlockwise, drives the internal threaded rod 402 to rotate along with the external transmission rod 401, and then the valve plate 403 moves upwards under the rotation drive of the internal threaded rod, so that the vacuum valve is opened.
In practical applications, the connection region 22 further includes a valveless cavity with at least three openings, as shown in fig. 11 and 12, and fig. 11 shows a valveless cavity with three openings, and fig. 12 shows a valveless cavity with four openings for connecting multiple feeding regions and collecting regions. As shown in fig. 2 and 3, a feeding area 21 is connected with a plurality of collecting areas 23 through a connecting area 22 with valves, the two ends of the collecting area are opened, a multi-stage purifying cavity is formed, all the connecting areas are fastened by vacuum flanges, then a finer temperature gradient is set through a background control system, the purity of target materials can be improved, and different target materials can be purified through different temperatures set in each collecting area.
Further, as shown in fig. 4, the multiple multi-stage purification cavities can be connected in parallel through multiple valveless cavity connection areas with four ends open as shown in fig. 12, so as to be used for purifying organic materials by large-scale sublimation.
Further, the invention also comprises a vacuumizing device for vacuumizing the integrated cavity.
The invention provides a modularized sublimation purification system, which can realize active temperature adjustment by arranging a heating wire inside a cavity wall and arranging a temperature sensor to transmit a temperature signal to a background control system; the vacuum valve is arranged on the connecting module, when the valve is closed, the feeding module and the collecting module can be separated independently, the feeding area and the collecting area are convenient to replace, and time is saved; the feeding area and the collecting areas are connected in series through the connecting modules, and a fine temperature interval is arranged in each collecting area, so that continuous sublimation and purification of raw materials can be realized to obtain high-purity target materials, and target materials with different sublimation temperatures can be purified; the plurality of feeding areas are connected with the plurality of collecting areas in series and parallel through the connecting module, large-scale sublimation purification can be achieved, the feeding areas are independent from the collecting areas due to the arrangement of the vacuum valves, target materials can be quickly changed or collected and taken out, consumed time is reduced, high-efficiency sublimation purification is achieved, and various purification requirements can be met.
It is to be understood that the invention is not limited in its application to the examples described above, but is capable of modification and variation in light of the above teachings by those skilled in the art, and that all such modifications and variations are intended to be included within the scope of the appended claims.

Claims (2)

1. The modularized sublimation purification system is characterized by comprising a feeding module, a collecting module, a connecting module, a heating module, a vacuumizing device and a background control system, wherein the feeding module is connected with the collecting module through the connecting module, the heating module is connected with the feeding module, the collecting module and the connecting module, the vacuumizing device is connected with the collecting module in series, and the heating module is connected with the background control system;
The feeding module comprises at least one feeding area, and the feeding area is a cavity with one end open;
The collecting module comprises at least one collecting area, and the collecting area is a cavity with two open ends;
The connecting module comprises at least one connecting area, the connecting area is a cavity with two open ends, the feeding area and the collecting area are connected in series through the connecting area to form an integrated cavity, the connecting areas are fastened through a vacuum flange, and a vacuum valve is arranged in the cavity of the connecting area;
the heating module comprises a plurality of groups of heating wires, and the start and stop of each group of heating wires are mutually independent and are used for heating the feeding module, the collecting module and the connecting module;
The vacuumizing device is used for vacuumizing the integrated cavity;
The background control system controls the temperature of the feeding module, the collecting module and the connecting module by controlling the heating module;
the heating module further comprises a plurality of temperature sensors, each group of heating wires corresponds to one temperature sensor, and the temperature sensors are used for sending temperature signals to the background control system;
A group of heating wires and corresponding temperature sensors are arranged in the cavity wall of the feeding area, and a group of heating wires and corresponding temperature sensors are arranged in the cavity wall of the collecting area; the inside condensation collection platform that is provided with of collection district, condensation collection platform inside sets up multiunit heater strip and corresponding temperature sensor, the vacuum valve will the connection district is one divides into two, set up a set of heater strip of mutually independent and corresponding temperature sensor in the connection district cavity wall of vacuum valve both sides respectively, the inside a set of heater strip and the corresponding temperature sensor that sets up of vacuum valve, the connection district still includes the valveless cavity of at least three terminal opening for connect a plurality of feed district and collection district, a feed district series connection a plurality of collection district, the series connection is through a plurality of both ends open-ended valve cavity connecting areas connection, and every collection district sets up different temperatures through backstage control system, constitutes the multistage purification cavity, and a plurality of multistage purification cavities are parallelly connected through a plurality of at least three terminal open-ended valveless cavity connecting areas for purifying organic material on a large scale sublimates.
2. A modular sublimation purification system as claimed in claim 1, wherein the feed zone cavity, the collection zone cavity and the connection zone cavity are made of aluminum alloy or stainless steel.
CN201811160080.1A 2018-09-30 2018-09-30 Modularized sublimation purification system Active CN108992962B (en)

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