KR102154843B1 - A sublimation purification apparatus for organic materials having replaceable purification unit - Google Patents

Abstract

The present invention relates to an organic substance sublimation and purification apparatus that performs a process for extracting pure organic substances by separating and removing impurities through sublimation and purification of organic substances, and in particular, by providing an organic substance purification unit to be replaced in a recovery unit It relates to an organic material sublimation and purification apparatus capable of increasing production efficiency by allowing sublimation recovery.

Description

Organic substance sublimation purification device with replaceable purification unit {A SUBLIMATION PURIFICATION APPARATUS FOR ORGANIC MATERIALS HAVING REPLACEABLE PURIFICATION UNIT}

The present invention relates to an organic substance sublimation and purification apparatus that performs a process for extracting pure organic substances by separating and removing impurities through sublimation and purification of organic substances. In particular, the sublimation recovery of the sublimation object can be continuously performed, thereby increasing production efficiency. It relates to an organic material sublimation purification device that can be.

As an image display device, the display is a display device for displaying result data processed by the information processing device as an image. Thanks to the technology development of modern information processing devices, such technology development is also rapidly progressing. A typical display device is an organic light generating device (OLED). The organic light generating device displays an image using an organic light emitting material that emits light.

In this case, the characteristics of the organic light generating device have a close relationship with the purity of the organic material constituting the organic light emitting layer. When the purity of the organic material is low, it is difficult to generate light of a desired color, and the display quality of the image is greatly reduced.

Therefore, the organic material sublimation purification apparatus is mainly used in the sublimation purification process, which is a process of removing impurities from organic materials used to form a light emitting layer or a transport layer of an organic EL or OLED panel.

In general, an organic material purification apparatus is used to heat and sublimate an organic material to separate impurities and obtain high-purity refined products. Such a sublimation purification apparatus is used in a sublimation purification process, which is a process for removing impurities of low molecular weight organic substances that can be used as light emitters or transporters of organic EL or OLED devices.

Therefore, conventionally, a lot of research has been conducted on the development of an organic substance sublimation and purification apparatus for purifying organic substances having high purity by removing impurities through such a process.

Referring to FIG. 1, a conventionally developed organic substance sublimation purification apparatus 1 largely sublimates and collects organic substances from a purification object M, and an outer pipe 40 including the inner pipe 50 ), a vacuum pump 20 provided on one side of the outer tube 40 to selectively control the vacuum state inside the inner tube 50 and a trap unit that blocks the sublimated organic matter from moving to a specific area do.

In the inner tube 40, a purification object is generally placed therein, and when heated by high heat, organic substances sublimate from the purification object M, and the sublimated organic substances move and are collected.

The vacuum pump 20 is connected in communication with one side of the outer tube 40 and controls the internal vacuum state, thereby controlling the interior of the inner tube 50 to a high vacuum state.

On the other hand, in a high vacuum state, the distribution of gas inside becomes extremely small, and accordingly, there is no gas flow.

Accordingly, in the inner tube 50, which is in a high vacuum state by the vacuum pump 20, organic substances sublimated therein freely move and are collected.

At this time, the doors 31 and 32 create a sealed space inside the inner tube 50, and organic substances or impurities in the vaporized state are attached to the inner surface of the vacuum chamber.

The inside of the outer tube 40 is formed as a vacuum chamber, and impurities are sublimated and purified by the heaters 60 located on the outer circumference of the outer tube 40 to adhere to the inner tube 50.

At this time, the heater 60 divides the region in the longitudinal direction and heats it to a plurality of high temperatures, and the impurities of the purification object M are sublimated according to the temperature. Therefore, the impurities are separated and removed at the designated temperature of each heater. You can do it.

However, in the case of such a conventional invention, the size of the purification object M placed in the inner tube 50 is inevitably limited, and the amount of the material to be purified by sublimation can only be about 3 kg at most.

If you want to obtain a large amount of purified product, a lot of work has to be performed, and quality degradation is also a concern by purifying a small amount. In order to improve productivity and quality, there is a need to improve the organic material sublimation purification device.

An object of the present invention is to solve the problems of the conventional organic substance sublimation and purification apparatus, and more particularly, the organic substance purification unit is coupled to the recovery unit while forming a vacuum chamber so that it can be replaced, so that the object to be purified can be continuously sublimated and recovered. Thus, it is to provide an organic substance sublimation and purification apparatus that can increase production efficiency.

In order to solve the above problems, the present invention is a purification unit having a predetermined length and having an object to be purified inside and heated by a purification heater unit to purify the object to be purified; and, an organic substance sublimated from the object to be purified to a recovery heater unit And a recovery unit that is heated to be collected according to temperature, wherein the purification unit is provided to be separated and replaced independently from the recovery unit.

In addition, the purification unit may include a first door that allows the object to be purified to be drawn in and out; and a second door that is coupled in communication with one side of the recovery unit to form a vacuum chamber, wherein the second door comprises: A first vacuum pump for forming a vacuum chamber in a high vacuum state inside the purification unit may be provided.

In addition, the purification unit may include a purification outer tube for maintaining a vacuum state therein; And a purification tube which locates the purification object and is drawn in and out of the purification outer tube in the longitudinal direction.

The recovery unit may include a third door for sealing a longitudinal end opposite to the purification unit; And a second vacuum pump for forming a vacuum chamber in a high vacuum state inside the recovery unit.

In addition, the recovery unit, a recovery outer pipe for maintaining a vacuum state therein; And an anti-seizure pipe attached to the impurities separated and extracted from the purification object and drawn in and out of the recovery outer pipe in the longitudinal direction.

In addition, the recovery heater unit is partitioned in a longitudinal direction into a plurality of temperature zones so that impurities can be attached according to the heating temperature, and the seal-proof tube can separate impurities to be attached and collected according to the temperature division of the recovery heater unit. I can.

In addition, the purification unit may be provided with a plurality of purification outer tubes so that they are continuously coupled to the first door and the second door to enable replacement.

Further, the purification unit may be provided integrally between the first door and the second door so that the recovery units are sequentially coupled to continuously sublimate and purify a plurality of purification targets.

In the present invention, the purification unit in which the purification object is located is sequentially and continuously formed and combined with a vacuum chamber in the recovery unit, so that a large amount of the purification object is continuously purified and recovered compared to the conventional single process, so that a much higher amount of organic matter purification yield Can be obtained, thereby contributing to productivity improvement.

In addition, in the present invention, since the purification operation of the purification object is performed by replacing only the purification unit of the organic substance sublimation purification apparatus, the efficiency of the operation can be achieved, and further, the operation speed can be improved to achieve more organic substances purification operation.

In addition, the present invention is a separate configuration of the refining unit and the recovery unit, so that when a failure or repair of each component is required, it is possible to easily separate and repair, thereby increasing the durability of the product.

1 is a view showing an organic material sublimation purification apparatus according to the prior art,
2 is a view showing an organic material sublimation purification apparatus having a replaceable purification unit of the present invention,
3 is a view showing that the purification unit of the present invention is replaced,
FIG. 4 is a view showing that a plurality of purification units are combined and replaced with a first door and a second door according to another embodiment of the present invention.
FIG. 5 is a diagram illustrating that a plurality of integrated purification units are sequentially combined with a plurality of vacuum chambers and a recovery unit formed of a first door and a second door as another embodiment of the present invention.

Hereinafter, preferred embodiments of the sublimation purification apparatus of the present invention will be described with reference to the accompanying drawings. In this process, the thickness of the lines or the size of components shown in the drawings may be exaggerated for clarity and convenience of description.

In addition, terms to be described later are terms defined in consideration of functions in the present invention and may vary according to the intention or custom of users or operators. Therefore, definitions of these terms should be made based on the contents throughout the present specification.

In addition, the following examples do not limit the scope of the present invention, but are merely exemplary matters of the elements presented in the claims of the present invention, and are included in the technical idea throughout the specification of the present invention and the composition of the claims. Embodiments including elements that can be substituted as equivalents in elements may be included in the scope of the present invention.

Hereinafter, a configuration and an embodiment of the present invention will be described with reference to FIGS. 2 and 3.

FIG. 2 is a view showing an organic substance sublimation purification apparatus having a replaceable purification unit of the present invention, and FIG. 3 is a view showing that the purification unit of the present invention is replaced.

In the present invention, unlike a conventional integrated organic substance sublimation and purification apparatus, the purification unit 200 and the recovery unit 300 are independently configured and operated.

Accordingly, the purification unit 200 has a separate first vacuum chamber P1, which is preferably formed by the first vacuum pump 240 connected to the second door 232.

The vacuum chamber P2 of the recovery unit 300 is formed by a second vacuum pump 340 that is normally connected to the third door 330 as in the conventional sublimation purification device, so that impurities N are prevented To be attached to (320).

The first vacuum chamber P1 and the second vacuum chamber P2 may be formed as separate vacuum pumps, each having the first vacuum pump 240 and the second vacuum pump 340 mentioned above. If it is difficult to employ a plurality of expensive vacuum pumps, it may be configured as a vacuum pump consisting of one set consisting of a low vacuum pump and a high vacuum pump.

Accordingly, the present invention may include a vacuum pump comprising a low vacuum pump and a high vacuum pump to form a vacuum chamber in a high vacuum state inside the purification unit and the recovery unit.

As such, the first vacuum pump 240 may be connected to and provided with the second door 232, as shown in FIGS. 2 and 3, but may form the first vacuum chamber P1. If there is a structure, the first vacuum pump 240 and the second vacuum pump 340 may be configured with the same pump, and any method other than this may belong to the scope of the present invention.

In addition, the first vacuum pump 240 may be connected between the first door and the second door to form a vacuum chamber in a high vacuum state inside the purification unit, and the second vacuum pump 340 is a second It is connected between the door and the third door, it may be provided to form a vacuum chamber in a high vacuum state inside the recovery unit.

As shown in FIG. 3, since the purification unit 200 and the recovery unit 300 can be independently combined, a large amount of purification targets (M) while sequentially combining a plurality of the purification units 200 Sublimation and purification process.

As shown in Fig. 2, the sublimation and stabilization apparatus 100 of the present invention has a predetermined length, and the purification object M is placed therein, and is heated by the purification heater unit 260 to purify the purification object M. It includes a purification unit 200, and includes a recovery unit 300 that allows the organic impurities N sublimated from the purification object M to be heated by the recovery heater unit 360 and collected according to the temperature.

Since the configuration and operation relationship of the purification unit 200 and the recovery unit 300 itself is similar to that of a conventional organic substance sublimation and purification apparatus, a detailed description will be omitted below.

The purification unit 200 of the present invention is characterized in that it is provided to be independently separated and replaced from the recovery unit 300.

The purification unit 200 includes a first door 231 that allows the object to be purified (M) to be drawn in and out, and a second door that is coupled to one side of the recovery unit 300 to form a vacuum chamber P1. (232) may be included.

The second door 232 of the present invention may include a first vacuum pump 240 forming a vacuum chamber P1 in a high vacuum state inside the purification unit 200. However, if the first vacuum pump 240 is a configuration capable of forming the first vacuum chamber P1, it may be connected to and installed in a configuration other than the second door 232, and the range possible to implement this embodiment. If so, it is considered to be within the scope of the present invention.

The refining unit 200 may include a refining outer pipe 210 for maintaining a vacuum state therein, and a refining pipe 230 for placing the object to be purified and drawing in and out of the refining outer pipe in a longitudinal direction.

The external purification tube 210 may perform its configuration and function in any form as long as it has a structure capable of maintaining a vacuum state inside the purification unit as in the configuration of a conventional organic substance sublimation purification device.

The refining pipe 230 is a part where the purification object M to be sublimated and purified by the present invention is seated, so that the refining unit 200 can be withdrawn into and out of the longitudinal direction.

Referring to FIGS. 2 and 3, the structure and operation relationship that can be independently separated and replaced is a vacuum chamber in which the purification unit 200 is a high vacuum space between the first door 231 and the second door 232. It is possible by forming P1), which is achieved by forming a high vacuum space through the first vacuum pump 240 in a state in which the purification unit 200 is hermetically coupled to the recovery unit 300 through the first door 231. .

The first vacuum pump 240 may be connected to and provided with the second door 232, as shown in FIGS. 2 and 3, but if it has a structure capable of forming the first vacuum chamber P1 Whatever method is employed, it may be included in the scope of the present invention.

The recovery unit 300 of the present invention collects the organic impurities N sublimated and purified from the purification target M, and may be configured in a plurality of two or more according to a temperature division.

Referring to FIG. 2, the recovery unit 300 includes a third door 330 sealing the longitudinal end opposite to the purification unit 200 and a vacuum chamber P2 in a high vacuum state inside the recovery unit 300. It may include a second vacuum pump 340 forming a.

The recovery unit 300 of the present invention attaches a recovery outer tube 310 for maintaining a vacuum state therein, and impurities N separated and extracted from the purification object M, and the inside of the recovery outer tube 310 It may include an anti-seal tube 320 that is drawn in and out in the longitudinal direction.

The recovery outer tube 310 functions the same as the outer tube configuration of a conventional organic substance sublimation and purification apparatus and maintains the inside of the recovery unit 300 in a vacuum state.

The recovery heater unit 300 may be divided in a length direction into a plurality of temperature regions so as to attach impurities according to the heating temperature, and may be provided in plurality.

The anti-stick pipe 320 separates and collects impurities (N) to be attached and collected according to the temperature division of the recovery heater unit 360, and the purification object (M) through the purification unit 200 which is sequentially replaced and combined. It becomes possible to continuously sublimate and stagnate the impurities (N) of.

According to another embodiment of the present invention, the first door 231 is provided so that the refinery tube 220 can be withdrawn in the interior of the refinery outer tube 210 in the longitudinal direction, and the second door ( 232 may be provided so that the refining pipe 220 or the anti-dissolving pipe 320 can be withdrawn in a longitudinal direction inside the refining outer pipe 210 or the recovery outer pipe 310.

In addition, the third door 330 is provided so that the room-proof tube 320 is provided in the inside of the recovery outer tube 310 so as to be able to be withdrawn in the longitudinal direction.

In this way, the present invention adopts a structure in which the purification unit 200 and the recovery unit 300 are independently drawn in and out through the first to third doors 231, 232, and 330 and can be combined, It is possible to purify the impurities (N) of high yield by increasing the efficiency of sublimation purification of the object to be purified (M).

Hereinafter, other embodiments of the present invention will be described with reference to FIGS. 4 and 5.

FIG. 4 is a view showing that a plurality of purification units are combined with a first door and a second door according to another embodiment of the present invention, and FIG. 5 is another embodiment of the present invention. It is a view showing that the plurality of vacuum chambers formed by the first door and the second door are sequentially combined with the recovery unit.

Referring to FIG. 4, a plurality of the purification units 200 are provided integrally between the first door 231 and the second door 232 so that the recovery unit 300 is sequentially coupled to a plurality of tablets. It makes it possible to continuously sublimate and purify the objects (M1 to M3).

This configuration and operation relationship allows the purification unit 200 to sequentially and smoothly continuously operate the sublimation purification operation, and each purification unit provided with the purification outer tubes 211, 212, 213 and the purification tubes 221, 222, 223 independently It is possible to form a high vacuum state within (200).

Looking at another embodiment of the present invention with reference to FIG. 5, the purification unit 200C includes a plurality of purification outer tubes 210C, and thus the first door 231C and the second door 232C They are continuously combined to allow replacement.

The refining unit 200C of FIG. 5 shows that the three outer refining pipes 210C and the refining pipe 220C are combined to form a large unit, but three are only one example, and the sublimation refining operation is smooth. If it is a condition that can be performed, a larger number of units can be formed.

Purification targets (M1 to M3) in the purification pipe (220C) are sequentially hermetically coupled to the recovery unit 300 through a second door (232C), so that the purification targets (M1 to M3) are sequentially sublimated and purified, resulting in many impurities. (N) can be recovered.

In this way, the plurality of refinery pipes (220C) are integrally combined with the refinery outer pipe (210C) to form one large unit, which improves durability and increases the productivity with a structure that can maximize work efficiency. There will be.

In this way, the present invention adopts a method that can continuously replace the refining unit part (Loading part), so that at least 3 kg (20 kg or more) in the limit of sublimation purification and recovery by putting up to 3 kg of material in the existing sublimation purification device. Possible) Sublimation purification and impurities can be recovered by continuously adding materials, and accordingly, the production efficiency of the sublimation purification apparatus is dramatically increased compared to the existing sublimation purification apparatus.

As described above, preferred embodiments of the present invention have been described, and in addition to the above-described embodiments, other forms may be embodied without departing from the spirit or scope of the present invention. Therefore, the present embodiment should be regarded as illustrative rather than restrictive to a specific form, and accordingly, the present invention is not limited to the above description and may be modified within the scope of the appended claims and equivalents thereof.

1: sublimation purification device according to the prior art 10: base
20: vacuum pump 31, 32: door
40: outer tube 50: inner tube
60: heater M: purification object
100: sublimation purification device according to the present invention 200: purification unit
210: refinery outer tube 220: refinery tube
231: first door 232: second door
240: first vacuum pump 260: purification heater unit
300: recovery unit 310: recovery outer pipe
320: anti-vibration pipe 330: third door
340: second vacuum pump 360: recovery heater unit
P1, P2: vacuum chamber N: impurities

Claims (11)

A purification unit having a predetermined length and having a purification object placed therein and heated by a purification heater unit to purify the purification object; And
A recovery unit for heating the organic matter sublimated from the purification object by a recovery heater unit to be collected according to temperature;
In the organic material sublimation purification apparatus comprising a,
The purification unit,
A purification outer tube for maintaining a vacuum state inside;
A purification tube which locates the purification object and is drawn in and out of the purification outer tube in a longitudinal direction;
A first door allowing the object to be purified to be withdrawn; And
And a second door coupled in communication with one side of the recovery unit to form a vacuum chamber,
The recovery unit,
A recovery outer pipe for maintaining a vacuum state inside;
An anti-seizure pipe attached to the impurities separated and extracted from the purification object and drawn in and out of the recovery outer pipe in a longitudinal direction; And
It includes a third door for sealing the end of the longitudinal direction opposite to the purification unit,
The organic substance sublimation purification apparatus, characterized in that provided so that the purification unit and the recovery unit can be separated and replaced independently of each other.
delete The method of claim 1,
And a vacuum pump comprising a low vacuum pump and a high vacuum pump to form a vacuum chamber in a high vacuum state inside the purification unit and the recovery unit.
The method of claim 1,
The second door,
And a first vacuum pump for forming a vacuum chamber in a high vacuum state inside the purification unit.
The method of claim 1,
The recovery unit,
And a second vacuum pump for forming a vacuum chamber in a high vacuum state inside the recovery unit.
The method of claim 5,
Including; a first vacuum pump connected between the first door and the second door to form a vacuum chamber in a high vacuum state inside the purification unit,
The second vacuum pump is connected between the second door and the third door to form a vacuum chamber in a high vacuum state inside the recovery unit.
delete The method of claim 1,
The recovery heater unit is partitioned in a longitudinal direction into a plurality of temperature zones so as to adhere impurities according to the heating temperature,
The deposition-proofing pipe is an organic substance sublimation purification apparatus, characterized in that the impurities to be attached and collected are classified according to the temperature division of the recovery heater unit.
The method of claim 1,
The first door is provided so that the refinery tube can be withdrawn in a longitudinal direction into the inside of the refinery outer tube,
The second door is provided to allow the refining pipe or the seal-proof pipe to be withdrawn in a longitudinal direction inside the refining outer pipe or the recovery outer pipe,
The third door is an organic material sublimation and purification apparatus, characterized in that provided so that the discharge-proof pipe is able to be withdrawn in a longitudinal direction inside the recovery outer pipe.
The method according to any one of claims 1, 3 to 6, 8, and 9,
The purification unit,
An organic substance sublimation and purification apparatus, characterized in that a plurality of external purification tubes are provided so that the first door and the second door can be continuously combined and replaced.
The method according to any one of claims 1, 3 to 6, 8, and 9,
The purification unit,
An organic substance sublimation purification apparatus, characterized in that a plurality of pieces are integrally provided between the first door and the second door so that the recovery units are sequentially combined to continuously sublimate and purify a plurality of objects to be purified.

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