KR20150065515A - An apparatus for purifying organic electroluminescence materials and a method therefor - Google Patents

Abstract

The present invention is designed to solve the problems in a conventional sublimation purification apparatus of an organic material. The purpose of the present invention is to perform purification treatment for an organic material in liquid state and each process in a simultaneous and parallel manner. The present invention performs purification treatment using an organic material in liquid state compared to a conventional sublimation purification apparatus of an organic material, thereby automatically transporting an object to be treated between each process. In addition, each process can be separately treated to enhance productivity and output of an organic material by a simultaneous and parallel process.

Description

FIELD OF THE INVENTION [0001] The present invention relates to an apparatus for purifying organic electroluminescent materials and a method for purifying organic electroluminescent materials,

The present invention relates to a liquid state refining apparatus and a refining method of an organic material for forming an organic electroluminescent material.

Organic materials conventionally used for organic electroluminescent devices require purification. The refining technology of the organic material is for separating only the components necessary for pure electroluminescence among the synthesized materials for use in thin film deposition. As the purification technology of the organic material is improved, the color purity and the luminous efficiency are improved, Extended life. In order to mass-produce organic materials, it is essential to shorten the process time and refine organic materials with improved purification efficiency.

A sublimation purification method of an organic material is disclosed in HJ Wagner, el al., Journal of Materials Science, 17, 2781, (1982), wherein a glass tube having a length of about 1 m is inserted into a thermoconductive copper tube, A sample of the organic material to be purified is arranged in the sub region once. A heater is attached to surround the copper tube around the sample of the organic material. The inside of the glass tube is maintained in a vacuum state, and the sample in the glass tube is heated by the heater to sublimate the molecule of the organic material of the sample. The glass tube has a temperature deviation, and the vapor of organic molecules is cooled and recrystallized in the other end region of the glass tube. As a result, recrystallized organic crystals are produced in the other end region of the glass tube.

Fig. 1 shows a conventional sublimation purification apparatus 100 for organic materials. In a conventional sublimation refining apparatus 100, an inner tube 10 for storing a raw material for producing an organic material used for an organic electroluminescence device, and an inner tube 10 for collecting purified materials for collecting the organic material purified in the sublimation refining step The inner tube 20 is used.

On the other hand, there is an outer tube 30 as a chamber in which the sublimation purification process of the organic material is performed, and the heater 40 surrounds the outer surface of the outer tube 30. The outer tube 30 may be divided into a plurality of regions, and each of the regions may be adjusted to a different temperature by the heater 40.

An inner tube 10 for storing a raw material and an inner tube 20 for collecting an empty refined material are placed in an outer tube 30 and then heated by a heater 40 Start heating. When the raw material is heated above the sublimation point, the raw material sublimes and becomes a gaseous state. At this time, if the area of the outer tube equipped with the refined material collecting inner tube 20 is heated to the sublimation point of the material to be obtained in the sublimation refining step by the heater 40, the refined material, And is formed into a solid state in such a manner as to surround the inner peripheral surface of the refined material collecting inner pipe 20.

In the conventional sublimation refining apparatus, a batch process is completed by charging a raw material which can be produced in batch type due to a restriction condition in the purification process, and then discharging the purified material through a purification process. Korean Patent Laid-Open Publication No. 10-2010-0114342 also refers to a sublimation purification apparatus and a sublimation purification method using the apparatus. However, the conventional sublimation purification apparatus and method as disclosed in the above-mentioned documents have a limitation in increasing the productivity and the production amount because the respective steps are carried out manually and sequentially.

Further, in the conventional sublimation refining apparatus, the raw material is melted during the step of heating the raw material in the solid state according to the diversity of the organic material, and thus there is a difficulty in the process management.

SUMMARY OF THE INVENTION The present invention has been made to overcome the above-described problems in a conventional sublimation purification apparatus for organic materials, and aims at purifying an organic material in a liquid state.

It is another object of the present invention to enable the respective steps to be carried out simultaneously and in parallel in the purification of organic materials.

An apparatus for purifying an organic electroluminescent material according to the present invention includes: a loading unit for heating a raw material in a solid state to convert the raw material into a liquid state; A refining unit for heating and purifying the liquid raw material by vaporization; And a collecting part for storing purified liquid purified in the purifying part.

Further, in the apparatus for purifying an organic electroluminescent material according to the present invention, the refining unit may include: a first chamber for heating and vaporizing the liquid raw material; And a second chamber in which the vaporized raw material is liquefied.

Further, in the apparatus for purifying an organic electroluminescent material according to the present invention, the loading section, the refining section, and the collecting section are formed using ceramics.

Further, in the apparatus for purifying an organic electroluminescent material according to the present invention, the second chamber is formed to have an inclined surface in which the purified purified liquid in the liquid flows inside and is led to the collecting part.

Further, in the apparatus for purifying an organic electroluminescent material according to the present invention, the refining unit may include a third chamber vertically formed between the first chamber and the second chamber, wherein the vaporized raw material drawn in the first chamber And the third chamber is drawn out to the second chamber after liquefaction and separation of the impurities during the ascending.

Further, in the apparatus for purifying an organic electroluminescent material according to the present invention, a connecting portion for allowing the liquid raw material to move in a hermetic state between the loading portion and the first chamber, wherein the connecting portion has a first A connecting portion; And a second connection portion between both the first connection portion and the loading portion and between the first connection portion and the first chamber to ensure a hermetic state at both ends thereof.

In addition, in the apparatus for purifying an organic electroluminescent material according to the present invention, the connection portion is formed to further include a valve for regulating the movement of the liquid state raw material between the loading portion and the first chamber.

In addition, in the apparatus for purifying an organic electroluminescent material according to the present invention, the connection portion may be further formed to include a fitting for mechanically coupling the first connection portion and the second connection portion.

The method for purifying an organic electroluminescent material according to the present invention comprises the steps of: heating a raw material in a solid state to convert it into a liquid state; Heating the liquid raw material to vaporize and purify the liquid raw material; And storing purified liquid refined material.

Further, in the method for purifying an organic electroluminescent material according to the present invention, the purifying step may include: a first purifying step of heating and vaporizing the liquid raw material; And a second purifying step in which the vaporized raw material is liquefied.

Further, in the method for purifying an organic electroluminescent material according to the present invention, the purifying step may include a third purifying step in which impurities are separated and separated while the raw material vaporized in the first purifying step rises along a vertical path, .

The present invention can carry out the transfer of the object to be processed between the respective processes automatically by using a liquid state organic material in comparison with a conventional sublimation and purification apparatus for an organic material. Further, each process can be separated and processed, and the productivity and the production amount of the organic material can be increased by a simultaneous and parallel process.

1 is a view showing a conventional sublimation purification apparatus for an organic material;
2 is a view showing an apparatus for purifying an organic electroluminescent material according to an embodiment of the present invention.
3 is a view showing an apparatus for purifying an organic electroluminescent material according to another embodiment of the present invention.
4 is a block diagram illustrating a method of purifying an organic electroluminescent material according to an embodiment of the present invention.
5 is a block diagram illustrating a method of purifying an organic electroluminescent material according to another embodiment of the present invention.

≪ Purification apparatus of organic electroluminescent material &

2 shows an apparatus for purifying an organic electroluminescent material according to an embodiment of the present invention.

2, the OLED device according to one embodiment of the present invention includes a loading unit 200, a refining unit 300, a collecting unit 400, a connection unit 500, and a vacuum line 600a , 600b.

The loading part 200 is filled with a raw material 110 in a solid state through an injection port formed in the upper part. The solid raw material 110 injected into the loading unit 200 is preheated before being transferred to the refining unit 300 and is converted into a liquid state. As a means for preliminary heating, a heating band (not shown) may be used to surround the loading unit 200. The temperature of the preheating may be above the melting point of the purified material contained in the raw material and below the breaking point.

The refining unit 300 includes a first chamber 310 and a second chamber 320. The raw material 120 in a liquid state preliminarily heated by the loading unit 200 is transferred to the lower portion of the first chamber 310 through the connection unit 500 and is stored. The liquid raw material 120 stored in the lower portion of the first chamber 310 is heated for vaporization. The temperature of the heating may be higher than the vaporization point of the purified material contained in the raw material and lower than the vaporization point of the impurities contained in the raw material. As the heating means of the first chamber 310, a heating mantle (not shown) may be used. The configuration of the second chamber 320 will be described later.

Here, the connection part 500 allows the liquid raw material to move in a hermetic state between the loading part 200 and the first chamber 310. The connecting portion has a first connecting portion 520 having flexibility at the center, a first connecting portion 520 and a loading portion 200 at both ends, and an airtight portion between the first connecting portion 520 and the first chamber 310 And second connection portions 510a and 510b for assuring the state of the first connection portion 510a and the second connection portion 510b.

The first connecting part 520 can withstand a high temperature and a reduced pressure state because heating is performed in the loading part 200 and the first chamber 310 and each process is performed in a reduced pressure state through the vacuum lines 600a and 600b So that it can be made of a flexible material. The first connection part 520 may be formed of a metal thread or a mesh structure made of SUS (Steel Use Stainless) so as to have airtightness and flexibility at the same time.

Since the loading part 200 and the first chamber 310 may be made of ceramic and the first connection part 520 may be made of metal, the second connection part 520 may be made of a metal having a different coefficient of thermal expansion, (510a, 510b) are formed to ensure airtightness when the liquid raw material formed by preheating in the loading section (200) moves. To this end, the second connections 510a and 510b may include an O-ring.

The connection part 500 may include a valve 530 to control the movement of the liquid raw material between the loading part 200 and the first chamber 310. In particular, the valve 530 may be formed between the second connection part 510a and the first connection part 520. Therefore, it is possible that each process can be performed separately, so that an organic material can be formed in parallel and simultaneously.

The connection part 500 may include a fitting 540 between the second connection part 510b and the first connection part 520. [ The fitting 540 is formed to mechanically fasten the second connection portion 510b and the first connection portion 520. [

The second chamber 320 may extend in the horizontal direction between the first chamber 310 and the collecting part 400. One side of the second chamber 320 is connected to the first chamber 310 so that the vaporized raw material flows in the first chamber 310 and the other side of the second chamber 320 is liquefied in the second chamber 320 The purified water 130 is formed to flow out to the collecting part 400. The internal temperature of the second chamber 320 can be kept below the condensation point of the purified water contained in the raw material. The second chamber 320 can be heated by the heating means. As the heating means, a heating band (not shown) may be used.

Here, the second chamber 320 may be formed to have an inclined surface 320a in which the purified liquid purified water flows inside thereof and is led to the collecting part 400. That is, as compared with the structure in which the liquid purified in the second chamber 320 flows in the collecting part 400 and is collected horizontally, the collected liquid can be easily and efficiently collected in the inclined surface structure.

The collector 400 is connected to the second chamber 320 to store purified liquid 130 purified in the second chamber 320.

The loading unit 200, the refining unit 300, and the collecting unit 400 described above are processed in a high-temperature and a low-pressure state in each unit process, so that they may be damaged if they are formed of a metal material. Accordingly, the loading unit 200, the refining unit 300, and the collecting unit 400 may be formed of a ceramic material so that reactivity with the organic material is low.

The loading unit 200, the refining unit 300, and the collecting unit 400 may be connected to the vacuum lines 600a and 600b. When the organic material is heated in the atmosphere, each process can be processed under reduced pressure to prevent the oxygen from reacting with the vaporized organic material to be burnt.

FIG. 3 shows an apparatus for purifying an organic electroluminescent material according to another embodiment of the present invention.

The apparatus for purifying organic electroluminescent material according to another embodiment of the present invention is similar to the apparatus for purifying organic electroluminescent material according to the embodiment of the present invention except for the configuration of the third chamber 1330, The explanation for the above will be briefly made.

3, the apparatus for purifying an organic electroluminescent material according to another embodiment of the present invention includes a loading unit 1200, a purification unit 1300, a collecting unit 1400, a connection unit 1500, and a vacuum line 1600a , 1600b.

The loading part 1200 is filled with a raw material 1110 in a solid state through an injection port formed in the upper part. The solid raw material 1110 injected into the loading section 1200 is preheated before being transferred to the purification section 1300 and is converted into a liquid state.

The refining section 1300 includes a first chamber 1310, a second chamber 1320, and a third chamber 1330. The raw material 1120 in a liquid state preliminarily heated by the loading unit 1200 is moved to the lower portion of the first chamber 1310 through the connection unit 1500 and is stored. The liquid raw material 1120 stored in the lower portion of the first chamber 1310 is heated for vaporization.

The third chamber 1330 may extend vertically between the first chamber 1310 and the second chamber 1320. The raw material heated and vaporized in the first chamber 1310 rises and flows into the second chamber 1320 through the third chamber 1330. Impurities contained in the vaporized raw materials other than the purified water pass through the third chamber 1330 and are liquefied and fall into a liquid state. Therefore, the purity of the purified product can be further increased by using the third chamber 1330.

Here, the connection part 1500 allows the liquid raw material to move in a hermetic state between the loading part 1200 and the first chamber 1310. The connecting portion has a first connecting portion 1520 having flexibility at the center and a first connecting portion 1520 and a loading portion 1200 at both ends and an airtight portion between the first connecting portion 1520 and the first chamber 1310 And second connection portions 1510a and 1510b for assuring the state.

The connection part 1500 may include a valve 1530 to control the movement of the liquid raw material between the loading part 1200 and the first chamber 1310.

The connection unit 1500 may include a fitting 1540 between the second connection unit 1510b and the first connection unit 1520.

The second chamber 1320 may extend in the horizontal direction between the first chamber 1310 and the collecting part 1400.

Here, the second chamber 1320 may be formed to have a sloped surface 1320a through which the purified liquid purified water flows inside thereof and is led to the collecting part 1400.

The collecting part 1400 is connected to the second chamber 1320 and stores purified liquid 1130 in a liquid state liquefied in the second chamber 1320.

≪ Purification method of organic electroluminescent material &

4 is a block diagram illustrating a method of purifying an organic electroluminescent material according to an embodiment of the present invention.

As shown in FIG. 4, the method for purifying an organic electroluminescent material according to an embodiment of the present invention includes a switching step (S100), a purification step (S200), and a storing step (S300). The purification step S200 includes a vaporization step S210 and a liquefaction step S220.

First, the raw material in a solid state is heated and converted into a liquid state (S100). The object to be treated can be automatically transferred between the respective steps by performing purification treatment using a liquid organic material in comparison with a conventional sublimation purification apparatus for an organic material. Further, each process can be separated and processed, and the productivity and the production amount of the organic material can be increased by a simultaneous and parallel process.

Next, the liquid raw material is heated to be vaporized and refined (S200). The purifying step includes a first purifying step (S210) of heating and vaporizing the liquid raw material, and a second purifying step (S220) in which the vaporized raw material is liquefied. In the first purification step (S210), the purified material contained in the raw material in the liquid state is vaporized, and the impurities can maintain the liquid state. In the second purification step (S220), the purified material contained in the vaporized raw material is liquefied, and the impurities can remain in the gaseous state. Gaseous impurities can be discharged using a vacuum line.

Next, the purified liquid state purified product is stored (S300). In the case of the conventional sublimation purification apparatus for organic materials, organic materials in a liquid state can be obtained in the present invention as compared with the case where recrystallized solid organic materials are collected. Therefore, when the organic EL device is manufactured through the deposition process after the purified organic material is changed to the gaseous state, further improved phase change efficiency can be obtained.

5 is a block diagram illustrating a method of purifying an organic electroluminescent material according to another embodiment of the present invention.

The method for purifying organic electroluminescent material according to another embodiment of the present invention is similar to the above-described method for purifying organic electroluminescent material according to one embodiment of the present invention except for the step of separating impurities (S2200) Briefly,

As shown in FIG. 5, the method for purifying an organic electroluminescent material according to another embodiment of the present invention includes a switching step (S1000), a purifying step (S2000), and a storing step (S3000). The purification step S2000 includes a vaporization step S2100, a separation step S2200, and a liquefaction step S2300.

First, the raw material in a solid state is heated and converted to a liquid state (S1000).

Next, the liquid raw material is heated to be vaporized and purified (S2000). The purifying step includes a first purifying step (S2100) for heating and vaporizing the liquid raw material, and a second purifying step (S2300) in which the vaporized raw material is liquefied.

Here, the method for purifying an organic electroluminescent material according to another embodiment of the present invention may further include a third purifying step (S2200) in which impurities contained in raw materials in a liquid state are separated by liquefaction and dropping. During the first purifying step (S2100), the impurities contained in the purified water other than the purified water are liquefied and fall into the liquid state during the rising of the vaporized raw material along the vertically formed passage, thereby further increasing the purity of the purified product.

Next, purified purified liquid is stored (S3000).

110: raw material in solid state 120: raw material in liquid state
130: Purified water in a liquid state 200: Loading section
300: refining unit 310: first chamber
320: second chamber 320a: inclined surface
400: collecting part 500: connecting part
510a, 510b: second connection part 520: first connection part
530: valve 540: fitting
600a, 600b: vacuum line 1110: solid material
1120: Liquid raw material 1130: Purified water in liquid state
1200: Loading section 1300: Purification section
1310: first chamber 1320: second chamber
1320a: inclined surface 1330: third chamber
1400: collecting part 1500: connecting part
1510a, 1510b: second connection portion 1520: first connection portion
1530: valve 1540: fitting
1600a, 1600b: vacuum line

Claims (11)

An organic electroluminescent material refining apparatus comprising:
A loading unit for heating the solid raw material to convert it into a liquid state;
A refining unit for heating and purifying the liquid raw material by vaporization; And
And a collecting section for storing purified liquid purified in the purifying section. The method according to claim 1,
The purification unit may include:
A first chamber for heating and vaporizing the liquid raw material; And
And a second chamber in which the vaporized raw material is liquefied. The method according to claim 1,
Wherein the loading section, the refining section, and the collecting section are formed using ceramics. 3. The method of claim 2,
The second chamber
Wherein the purified liquid state purified water flows inside and has an inclined surface leading to the collecting part. 3. The method of claim 2,
The purification unit may include:
And a third chamber vertically formed between the first chamber and the second chamber, wherein the vaporized raw material drawn in the first chamber is drawn out to the second chamber after liquefaction and separation of the impurities during the rising of the vaporized raw material, And further comprising a third chamber. The method according to any one of claims 2 and 4 to 5,
A connecting portion for allowing the liquid raw material to move in an airtight state between the loading portion and the first chamber,
A first connection part having flexibility; And
Wherein the first connection portion and the second connection portion are provided at both ends with a second connection portion between the first connection portion and the loading portion and between the first connection portion and the first chamber to ensure a hermetic state, Refining device. The method according to claim 6,
The connecting portion
Further comprising a valve for regulating the movement of the liquid state raw material between the first connection portion and the second connection portion. The method according to claim 6,
The connecting portion
Further comprising a fitting for mechanically coupling the first connection portion and the second connection portion. A method for purifying an organic electroluminescent material, comprising:
Heating the raw material in a solid state to convert it into a liquid state;
Heating the liquid raw material to vaporize and purify the liquid raw material; And
A method for purifying an organic electroluminescent material, comprising the steps of: storing purified liquid purified water. 10. The method of claim 9,
In the purification step,
A first purification step of heating and vaporizing the liquid raw material; And
And a second purification step in which the vaporized raw material is liquefied. 11. The method of claim 10,
In the purification step,
Further comprising a third purifying step of liquefying and separating the impurities while rising along the passage in which the raw material vaporized in the first purifying step is formed vertically.

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