TWI487566B - The method of refining organic materials with impurities through ionic liquids and apparatus therefore - Google Patents

Description

Organic material purification method and purification device using ionic liquid

The present invention relates to an organic material purification method and a purification apparatus based on an ionic liquid technology, and more particularly to a device for screening an optimal extraction combination between an ionic liquid (Ionic liquids) and an organic material of a purified article, even if a trace amount is used. OLED (Organic Light Emitting Diodes) organic materials, can also be used to quickly confirm which ionic liquid is most suitable for the organic material recrystallization of the material, simple purification method and purification device.

In addition, the present invention also relates to an organic material purification method and a purification apparatus capable of using a ionic liquid as a screening program to mass-purify an OLED organic material.

Recently, OLED display devices have been attracting attention as next-generation display devices. The reason for this is that not only the high driving voltage required for the inorganic LED is not required, but also the advantages of self-luminescence, flakes, fast response time, wide viewing angle, and the like, and the advantage that various organic compounds are easily colored. Such an OLED refers to a light-emitting element in which holes and electrons are recombined in an illuminating layer to form an exciton in an excited state, and light of a specific wavelength is emitted from the energy of the formed exciton.

Figure 1 is a conceptual diagram showing the structure of an OLED. As shown in FIG. 1, the OLED is formed by sequentially forming an anode (Anode) 120, a hole injection layer (HIL) 130, and a hole transport layer on a transparent substrate 110 such as glass. : HTL) 140, an organic light-emitting layer (EML) 150, an electron transport layer (ETL) 160, an electron injection layer (Electron injection layer: EIL) 170, and a cathode (Cathode) 180 .

An OLED in which a multilayer structure as described above is produced requires an organic substance for emitting light and transferring charges. However, because this organic matter not only interferes with the injection of electrons and electricity, but also directly interferes with the recombination of holes and electrons, the purity of organic matter is a very important factor affecting the color, luminous efficiency and lifetime of OLEDs. That is, a small amount of impurities in the organic matter is not only an increase in the probability of extinction of the injected charge, a decrease in the recombination probability of holes and electrons, but a decrease in luminous efficiency, and a new energy level due to the addition of impurities is a factor that lowers the purity of the luminescent color.

Therefore, in order to complete an electric field light-emitting element having high luminance, high efficiency, and long life, it is necessary to optimize the structure of the electric field light-emitting element, develop a new material with good hole (or electron) injection and transmission characteristics, and develop a new material for the organic light-emitting layer. Within, there is a need to increase the purity of OLED organics.

On the other hand, purification of OLED organics typically utilizes a recrystallization or sublimation recrystallization process of the solvent. The recrystallization method of sublimation is to recrystallize the organic material under vacuum, so that it has the property of not containing impurities. Therefore, a method of purifying an organic material of an organic electric field light-emitting element generally employs a sublimation purification method.

Here, sublimate refers to the migration phenomenon of a gas-solid phase generated at a temperature and pressure below the triple point of the phase equilibrium diagram. Even if the substance which is heated and decomposed under normal pressure is maintained at a low temperature below the triple point, it does not decompose at a higher temperature. With this property, in a sublimation device capable of controlling the temperature slope, an operation of heating the mixture to separate the impurities from the different sublimation points in a state in which the substance has not been decomposed is referred to as a vacuum sublimation method. This vacuum sublimation method is a purely physical method, and has the advantages of no reagent contamination and high resolution because it does not use a supplementary reagent or the remaining chemical methods, and is a useful method for purification of OLED organic materials.

At present, the purification method of the commonly used OLED organic material is a train sublimation purification method. In this method, the purified material is placed at the end of the hollow long tube, and the inside of the tube is evacuated by a vacuum pump, and the tube is heated by the heater to form a temperature gradient across the tube. Thus, depending on the material to be separated and the sublimation point of the impurity, the material can be separated by the difference in recrystallization position. Depending on the situation, nitrogen or an inert gas that does not react with the material constituting the purification device flows as a transport gas for transporting the organic material gas, from a high temperature to a low temperature, in a range where the degree of vacuum does not decrease much. This transport gas acts as a smooth flowing organic material gas.

Fig. 2 is a view schematically showing the configuration of a sublimation purification apparatus according to the prior art for performing a continuous sublimation purification method. As shown in Fig. 2, the organic material is placed in the crucible 240, and the crucible 240 is placed on the inner side of the second quartz glass tube 210. On the other hand, the outer side of the second quartz glass tube 210 is a structure in which the first quartz glass tube 220 is surrounded. Here, although the crucible 240 is not shown, it is configured to fit right at both end portions of the hollow cylindrical quartz tube at the open end portions, and is made of a stainless steel material, and has a pair of perforated covers.

The heater 250 is disposed around one side of the first quartz glass tube 220. At this time, the heater 250 is disposed at a position corresponding to the position of the crucible 240. The vacuum pump 230 is provided on the other side of the second quartz glass tube 210, and functions to maintain the vacuum state inside the second quartz glass tube 210.

In the sublimation purification apparatus 200 having the above configuration, first, the inside of the second quartz glass tube 210 is evacuated by the vacuum pump 230, and a small amount of transport gas flows to the entire second quartz glass tube 210 provided with the vacuum pump 230 to form a fine Pressure slope. Further, the temperature gradient of the entire second quartz glass tube 210 is gradually heated by the heater 250, and the temperature distribution formed at this time shows the shape of the normal distribution curve.

In addition, when the temperature of the crucible 240 is higher than the sublimation point of the raw material of the organic material contained in the purified material, the material begins to sublimate, and after the gas molecules formed at this time flow out to the outside of the crucible 240, the pressure slope is started to be set. The direction of the vacuum pump 230 moves. At this time, impurities higher than the sublimation point of the organic material raw material are retained inside the crucible 240.

The gas molecules in the direction in which the vacuum pump 230 is moved are further migrated to the solid phase in the second quartz glass tube 210 having the temperature lower than the sublimation point, and crystals are formed on the inner surface of the second quartz glass tube 210. Reference numeral 260 denotes a purified material which is formed in a crystal state on the inner surface of the second quartz glass tube 210. Further, after a certain period of time, the heating was stopped and the temperature was gradually cooled to room temperature, and the second quartz glass tube 210 was unwound and the purified material 260 in a crystalline state was recovered.

However, the organic material (extracting material) used in the OLED must be in a highly pure state in which the impurity content is extremely small, so that it is difficult to obtain a material of a desired purity by one-time purification. Therefore, the purification method using the apparatus shown in Fig. 2 requires repeated sublimation purification processes to obtain a high-purity material, and the repeated purification process requires a long operation time and is not suitable for mass production.

In addition, since the multi-step sublimation purification procedure is required, only a purification amount of 70% or less of the initial input organic material can be obtained, which has a problem of high cost and high power consumption.

In other words, the sublimation purification method is an example. Although there is an advantage that the raw material can be purified into a high-purity organic substance by utilizing the difference in sublimation point of the organic material, the purification process has a considerable amount of organic matter and inertness in the process of repeated sublimation-condensation. The gas is discharged together and lost, and there is a problem that the yield of the final purified material is very low compared to the starting material. In addition, there is a problem in that it takes a lot of time and expense to optimize the storage of the device according to each organic material.

In order to solve the above problems, the present inventors have provided that the ionic liquid which can be used in a vacuum can be used as a solvent to rapidly optimize the purification procedure parameters based on the ionic liquid program by the purification temperature of the selected organic material, the most suitable ionic liquid, and the like. A new organic material purification program based on an ionic liquid program capable of purifying OLED organic materials in large quantities.

However, since the price of the raw material of the OLED organic material is too expensive, it is necessary to experiment with a large number of purification procedures based on the ionic liquid program, which has practical obstacles such as cost. Therefore, it is necessary to quickly confirm whether the sublimation gas of the target organic material is recrystallized by using various ionic liquids as an object, and to study the temperature, pressure conditions and solubility changes of the recrystallized ionic liquid. Etc., a simple purification device that explores the possibilities of new purification procedures and optimizes program conditions. Thus, it is expected to save the program cost of a new large-scale purification program based on the ionic liquid program, and the effect of saving the time required for optimizing the program.

(The problem that the invention needs to solve)

Accordingly, the present invention has been made to solve the above-mentioned problems of the prior art, and an object thereof is to provide a process for confirming the purification of an organic material by experimentally recrystallizing a small amount of an organic material by using an ionic liquid which is stable in a vacuum. A simple purification method and a purification device for an organic material using an ionic liquid.

In addition, another object of the present invention is to provide an organic material purification method and a purification apparatus using an ionic liquid, which can conveniently mass-purify an OLED organic material by using an ionic liquid which is stable in a vacuum as a screening program.

(Technical means to solve the problem)

In order to accomplish the object as described above, a simple purification method of an organic material using an ionic liquid according to the present invention is a purification method for purifying an OLED (Organic Light Emitting Diodes) organic material by using an ionic liquid in a vacuum atmosphere, comprising: containing impurities a sublimation step of sublimation of the OLED organic material; a step of dissolving the diffused gas of the organic material dissolved in the ionic liquid; and supersaturating the organic material in the ionic liquid, thereby recrystallizing the organic material The recrystallization step.

Further, according to the invention, the organic material is sublimated by heating in the sublimation step.

Further, according to the invention, the ionic liquid is coated on a substrate, and in the dissolving step, in order to adjust the solubility of the organic material, the temperature of the substrate is adjusted.

Further, according to the invention, it is characterized in that the temperature of the substrate is maintained in the range of room temperature to 200 ° C in the dissolving step.

In addition, in order to accomplish the object as described above, the simple purification apparatus for an organic material using an ionic liquid according to the present invention, as an apparatus for purifying an organic material of an OLED (Organic Light Emitting Diodes) by using an ionic liquid in a vacuum atmosphere, comprises: containing impurities Sublimation means for sublimation of the OLED organic material; a sublimation gas of the diffused organic material dissolved in the ionic liquid to supersaturate the organic material, thereby recrystallizing the organic material.

Further, according to the present invention, the sublimation means includes: a crucible containing the organic material; a processing chamber provided with the crucible and having a certain internal volume; and evacuating the inside of the processing chamber a vacuum pump in a state; and a first heater that heats the crucible.

Further, according to the present invention, the sublimation means further includes a shutter that selectively opens or closes an upper side of the crucible.

Further, according to the present invention, the recrystallization means includes: a substrate on which the ionic liquid is applied; a shield that supports the substrate; and a portion that is heated on the substrate at an upper portion of the processing chamber a heater; and a support member formed to support the shield at a lower portion of the second heater.

Further, according to the present invention, the recrystallization means further includes a thermocouple provided on the support member to measure the temperature of the substrate, and the second heating is controlled by a temperature measured by the thermocouple. Temperature of the device.

Further, according to the invention, the ionic liquid is applied onto the substrate in the form of a droplet.

Further, according to the present invention, there is further provided an analysis means for photographing and analyzing the recrystallized organic material.

Further, according to the invention, the analysis means includes a thickness monitor for measuring the thickness of the recrystallized organic material.

In addition, in order to accomplish the object as described above, the method for purifying an organic material using an ionic liquid according to the present invention as a method for purifying an organic material of an OLED (Organic Light Emitting Diodes) by using an ionic liquid in a vacuum atmosphere includes: containing impurities a sublimation step of sublimation of the OLED organic material; a flow step of contacting the sublimation gas of the organic material to contact the ionic liquid; a step of dissolving the sublimation gas in the dissolution of the ionic liquid; and a step of dissolving the organic liquid in the ionic liquid The material is supersaturated, thereby recrystallizing the organic material.

Further, according to the present invention, in the flowing step, the sublimation gas is forcibly flowed by the inert gas into the ionic liquid stored in the storage tank.

Further, according to the present invention, the dissolving step and the recrystallization step further include discharging the inert gas which is not dissolved and collected in the upper portion of the storage tank to the outside of the storage tank Discharge step.

Further, according to the present invention, the recrystallization step further includes a recovery step of recovering the recrystallized organic material from the ionic liquid.

Further, according to the present invention, the heating step of heating the sublimation gas to maintain the temperature above the sublimation point of the organic material before the sublimation gas is mixed into the ionic liquid.

Further, according to the present invention, in the dissolving step, the temperature of the ionic liquid is adjusted in order to adjust the solubility of the organic material.

Further, according to the invention, the inert gas discharged in the discharging step is a carrier gas which is recycled as the flow step.

In addition, in order to accomplish the object as described above, an organic material purification apparatus using an ionic liquid according to the present invention, as an apparatus for purifying an OLED (Organic Light Emitting Diodes) organic material by using an ionic liquid in a vacuum atmosphere, includes: containing impurities a sublimation means for sublimating an OLED organic material; a means for flowing a sublimation gas flowing the organic material to contact the ionic liquid; and dissolving the sublimation gas in the ionic liquid to supersaturate the organic material, thereby Recrystallization means for recrystallization of materials.

Further, according to the present invention, the sublimation means includes: a crucible containing the organic material; a processing chamber provided with the crucible and having a certain internal volume; and evacuating the inside of the processing chamber a vacuum pump in a state; and a first heater that heats the crucible.

Further, according to the present invention, the recrystallization means includes: a storage tank for accommodating the ionic liquid; one side communicating with the inside of the processing chamber; and the other side immersing the ionic liquid in the storage tank a connecting conduit; and a vacuum pump that draws the interior of the storage tank into a vacuum state.

Further, according to the invention, there is further provided a second heater for heating the outside of the connecting duct in order to maintain the sublimation point of the organic material.

Further, according to the present invention, the third heater for heating the lower portion of the storage tank containing the ionic liquid in order to adjust the solubility of the organic material is further included.

Further, according to the present invention, it is characterized in that it further comprises an inner side upper portion of the storage tank, and the ionic liquid used for purification of the organic material is heated in a vacuum to a certain temperature or more and evaporated to collect Ionized liquid collection unit utilized.

Further, according to the present invention, the ionic liquid collecting portion includes: a collecting plate fixed to an inner side surface of the storage tank; and an ionic liquid collected on the inner side of the storage tank to collect the ionic liquid collected by the collecting plate Collect buckets.

Further, according to the present invention, there is further provided an ionic liquid retreating means for returning the ionic liquid collected by the collection tub to the storage tank.

Further, according to the present invention, there is further provided a recovery tank which is selectively connected to the storage tank and configured to be capable of being combined and separated to individually recover the recrystallized organic material.

Further, according to the present invention, the flow means includes an inert gas supply source for supplying an inert gas to one side of the processing chamber, and the recrystallization means further includes ions to be used in the storage tank A discharge pump that discharges the inert gas above the liquid to the outside of the storage tank.

Further, according to the present invention, the present invention further includes an inert gas retracting means for returning the inert gas discharged through the discharge pump to the inert gas supply source.

(cf. the efficacy of prior art)

According to the present invention, even if a trace amount of an organic material is sublimated, recrystallization can be confirmed in an ionic liquid, and therefore it is easy to confirm the possibility of purification of an organic material with a trace amount of an organic material.

Further, in the present invention, since the ionic liquid is non-volatile, the sublimation gas of the organic material is easily supersaturated in a trace amount of the ionic liquid, whereby the recrystallization process of the organic material can be quickly confirmed.

In addition, the present invention is a very simple construction of the apparatus, and even if the organic materials are different, there is an advantage that the cost and time required to explore the best ionic liquid and optimize the process conditions can be saved.

In addition, the present invention is a liquid screening method in which a sublimation gas generated in a sublimation purification process of an organic material is mixed in an ionic liquid which is stable in a vacuum, and the ionic liquid is used as a sublimation gas, thereby having a substantial increase in organic The advantage of the purified yield of the material.

Further, the present invention is an adjustment device having a large amount of ionic liquid, and the organic material is introduced into the ionic liquid to the supersaturation limit, whereby the organic material can be purified in a large amount, and the organic material can be reduced in cost.

Further, the present invention can be recycled by the re-purification procedure of the ionic liquid, thereby having the advantage that the manufacturing process can be greened.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, preferred embodiments of an organic material purification method and a purification apparatus using an ionic liquid according to the present invention will be described in detail with reference to the accompanying drawings.

<First Embodiment>

Fig. 3 is a perspective view showing the relationship of the constitution of an organic material simple purification apparatus using an ionic liquid according to the first embodiment of the present invention. As shown in FIG. 3, the organic material simple purification device 300 according to the present embodiment is a device for purifying an OLED organic material by using an ionic liquid in a vacuum atmosphere, comprising: a sublimation means for sublimating an OLED organic material containing impurities; and a diffused organic A recrystallization method in which a sublimation gas of a material is dissolved in an ionic liquid to supersaturate an organic material, thereby recrystallizing the organic material. In addition, the organic material simple purification device 300 according to the present embodiment further comprises: an analysis means for photographing and analyzing an organic material recrystallized in an ionic liquid; and controlling the sublimation means, the recrystallization means, and the analysis means as a whole Control means of operation.

The ionic liquid according to the present embodiment can utilize 1-Butyl-3-methylimidazorium bis(trifluoromethyl sulfonyl)imide (BMIM) of Chemical Formula 1. TFSI), or 1-octyl-3-methylimidazorium bis(trifluoromethyl sulfonyl)imide (OMIM TFSI) of Chemical Formula 2. Alternatively, 1-Ethyl-3-methylimidazorium bis(trifluoromethyl sulfonyl)imide (EMIM TFSI) can also be used.

Chemical formula 1

Chemical formula 2

The ionic liquid (BMIM TFSI, OMIM TFSI, EMIM TFSI) as described above is a non-volatile organic solvent. In the process of repeated dissolution-recrystallization of organic substances and impurities in an ionic liquid, the supersaturation is first achieved. The mechanism of recrystallization of organic materials can be used for purification and recrystallization of various organic materials.

On the other hand, BMIM TFSI, OMIM TFSI, EMIM TFSI has a low melting point, a low vapor pressure, a nonflammable, a consist of organic molecular ions, a cation and Characteristics such as controllable properties by combinations of anions and cations.

The ionic liquid according to the present embodiment is used for purification and recrystallization of an organic material, and can be stabilized in a liquid phase at 100 to 120 ° C, 10 ^-7 Torr, or as a solvent in a vacuum.

On the other hand, as the raw material of the organic material according to the present embodiment, NPB (N, N'-bis(naphthalen-1-yl)-N, N'-bis (phenyl) as a hole transport layer (HTL) material can be used. )-benzidine) material. Here, the sublimation point of NPB is 180 ° C or more. Therefore, when the crucible in the processing chamber constituting the sublimation means is heated to 200 ° C or more, sublimation is started.

On the other hand, the deposition material (organic material raw material) used for the production of the OLED element is various in addition to the materials as described above. Therefore, the present invention can use these different kinds of organic materials as raw materials.

Hereinafter, the bonding relationship between the constituent elements of the organic material simple purification device 300 according to the present embodiment will be described in detail.

The sublimation means is a crucible 320 containing a raw material 321 of an organic material containing impurities; a processing chamber 310 having a crucible 320 on one side and having a certain internal volume; and a vacuum pump for evacuating the inside of the processing chamber 310 (not shown) A first heater 322 that heats the crucible 320; and a shutter 340 that selectively opens or closes the upper side of the crucible 320.

Here, the shutter 340 may be configured to cover the upper end of the crucible 320, but is preferably covered with a certain distance from the upper end of the crucible 320. The control function of the shutter 340 is such that the sublimation gas of the organic material sublimated as the enthalpy 320 is heated is simultaneously moved to the recrystallization means in accordance with the diffusion phenomenon in the vacuum.

The recrystallization means is disposed at a position opposite to the crucible 320 inside the processing chamber 310 to recrystallize the sublimation gas of the organic material in the ionic liquid, and is supported by the crucible substrate 330 coated with the ionic liquid 331 to support the crucible substrate 330. The plate 333 is provided with a second heater 332 fixed to the upper portion of the processing chamber 310, a support member 334 formed on the lower support plate 333 of the second heater 332, and a thermocouple provided on the support member 334 for measuring the temperature of the substrate 330. 335 (thermocouple).

Here, the ionic liquid 331 is coated on the ruthenium substrate 330 in the form of a droplet. On the other hand, the thermocouple 335 measures the actual temperature of the crucible substrate 330, that is, the actual temperature permeation control means of the crucible substrate 330 is used to adjust the temperature of the second heater 332 based on the temperature applied by the second heater 332.

The analysis means is a purification material which is recrystallized in the ionic liquid 331 by photographing and analysis, and has a thickness monitor 350 or the like.

The function of the control means is to control the temperature of the first heater 322, the operation of the shutter 340, the temperature of the second heater 332 of the recrystallization means, and the operation of the analysis means as a whole.

Hereinafter, a method of purifying an organic material using the organic material simple purification apparatus of the present embodiment configured as described above will be described.

Fig. 4 is a flow chart showing a purification method using an organic material simple purification apparatus using an ionic liquid shown in Fig. 3. As shown in FIGS. 3 and 4, first, a crucible 320 containing an organic material raw material 321 is provided inside the processing chamber 310, and an upper portion of the crucible 320 is closed with a shutter 340, and the processing chamber 310 is treated by a vacuum pump. The inside is evacuated (S410).

Next, the first heater 322 is used to desorb the crucible 320 to the sublimation point of the organic material. Then, it becomes a sublimation gas of an organic material in which an organic material and a part of impurities are mixed (S420). The sublimation gas of such a sublimated organic material is gradually gathered by the shutter 340 at the upper portion of the closed crucible 320.

Then, when the shutter 340 is opened after a certain period of time, the sublimation gas of the organic material diffuses and moves toward the crucible substrate 330 by its own propulsive force, and the sublimation gas of the organic material is deposited on the ionic liquid 331. Then, the sublimation gas of the organic material contacts the ionic liquid 331 coated on the ruthenium substrate 330, is dissolved in the ionic liquid 331, and is recrystallized into an organic material (S430, S440). In other words, when the sublimation gas of the organic material dissolved in the ionic liquid 331 is supersaturated, it is recrystallized into an organic material to precipitate a highly purified material.

At this time, it is preferable that the temperature of the ruthenium substrate 330 is maintained in the range of room temperature to 200 °C. The reason for this is that an ionic liquid is exemplified, and a polymer material composed of elements of C, H, F, N, and O exists in an ion form, and has a characteristic that a high molecular structure is destroyed at a high temperature and the original property cannot be maintained. That is, although there is a slight difference between the ionic liquids, the characteristics are changed at about 200 ° C, so the use temperature range of the ionic liquid is limited to room temperature to 200 ° C. That is, in the range where the characteristics of the ionic liquid do not change, the temperature of the ionic liquid is increased by supersaturating the organic material through the ruthenium substrate 330, and when it is lower than room temperature, a sufficient amount of the organic material cannot be dissolved, and the organic material cannot be recrystallized. .

On the other hand, information on the purified material deposited in the ionic liquid 331 can be confirmed from the thickness measuring device 350. In addition, the precipitated high purity purified material can be appropriately recovered from the processing chamber 310.

Therefore, the present invention can be easily carried out, an experiment of sublimating a trace amount of an organic material and dissolving it in the ionic liquid 331 and recrystallizing it, and can be applied to a mass purification apparatus using an organic material of an ionic liquid.

<Second embodiment>

Fig. 5 is a conceptual diagram showing the relationship of the constitution of an organic material purifying apparatus using an ionic liquid according to a second embodiment of the present invention. As shown in FIG. 5, the organic material purification device 500 of the present embodiment includes: a sublimation means for sublimating an OLED organic material containing impurities; a flow means for contacting a sublimation gas of the flowing organic material to contact the ionic liquid; and dissolving the sublimation gas in the The crystallization liquid re-saturates the organic material, thereby recrystallizing the organic material. Further, the configuration of the organic material purification device 500 of the present embodiment further includes a control means for controlling the operation of the sublimation means, the flow means, and the recrystallization means.

Here, the sublimation means includes: a crucible 510 containing an organic material raw material 511; a processing chamber 520 provided with a crucible 510 and having a certain internal volume; a vacuum pump 550 that evacuates the inside of the processing chamber 520 into a vacuum state; The first heater 512 heated by the crucible 510 is configured. Further, the flow means includes an inert gas supply source 560 that supplies an inert gas to the side connected to the processing chamber 520.

Further, the recrystallization means includes: a storage tank 540 for accommodating the ionic liquid 541; a connection conduit 530 which is in communication with the inside of the processing chamber 520 on one side and immersed in the storage tank 540 on the other side; and an inside of the storage tank 540 The vacuum pump 550 which is evacuated and the discharge pump 553 which discharges the gas collected on the ionic liquid 541 of the storage tank 540 to the outside of the storage tank 540 are constituted.

On the other hand, the processing chamber 520 and the storage tank 540 are connected to each other on the upper side, and a vacuum pump 550 is provided at a joint portion thereof. Further, valves 551 and 552 that selectively communicate with the processing chamber 520 and the storage tank 540 are provided on the connection line of the vacuum pump 550, respectively.

Further, on the upper side of the storage tank 540, an ionic liquid 541 used for purification of an organic material may be collected to be collected by the ionic liquid collecting portion 570 which can be recovered by a purification procedure.

The ionic liquid 541 and the organic material raw material 511 used in the present embodiment are the same as in the first embodiment.

The crucible 510 is provided on the bottom surface side of the processing chamber 520, and has a first heater 512 at its lower portion. Further, the inside of the crucible 510 is configured to be capable of accommodating the raw material 511 of the purified material.

On the other hand, the connection duct 530 is disposed in such a manner that one side thereof is connected to the upper portion of the processing chamber 520, and the other side is extended through the upper portion of the storage tank 540, and is immersed in the ionic liquid 541. A second heater 531 that heats the connection duct 530 may be provided around the connection duct 530. Here, the second heater 531 functions to mix the mixed gas passing through the connection duct 530 into the ionic liquid 541, and to heat the periphery of the connection duct 530 so that the mixed sublimation gas 513 can maintain the sublimation point.

Further, a third heater 542 may be provided in the lower portion of the storage tank 540. Here, the third heater 542 functions to heat the ionic liquid 541 and adjust the solubility of the mixed sublimation gas 513 in the ionic liquid 541. Further, a discharge pump 553 may be provided on the upper side of the storage tank 540. At this time, it is preferable to provide the valve 554 on the line of the discharge pump 553.

Further, an ionic liquid collecting portion 570 may be provided on the upper side of the storage tank 540. Here, the ionic liquid collecting portion 570 functions to evaporate the ionic liquid 541 used in the purification of the organic material, and collect it so as to be recovered after the purification process of separating the impurities and the dissolved organic material, and the composition includes: fixing in the storage The inner side surface of the groove 540 has a collecting plate 571 having a curved surface shape, and is fixed to the inner side surface of the storage tank 540, and collects the collecting tank 572 of the ionic liquid collected by the collecting plate 571.

A method of purifying an organic material using the organic material purifying apparatus of the present embodiment constructed as described above will be described below.

Fig. 6 is a flow chart showing the purification method using the organic material purifying apparatus using the ionic liquid shown in Fig. 5. As shown in FIGS. 5 and 6, first, a crucible 510 containing an organic material raw material 511 is disposed inside the processing chamber 520, and after an appropriate amount of the ionic liquid 541 is injected into the storage tank 540, the processing chamber 520 is processed by a vacuum pump 550. And the storage tank 540 is evacuated. Then, the crucible 510 is heated by the first heater 512 to the sublimation point of the organic material. A mixed sublimation gas 513 of an organic material in which an organic material and a part of impurities are mixed is produced (S610).

In this state, the inert gas supply source 560 supplies an inert gas to the inside of the processing chamber 520. At this time, nitrogen or argon gas which does not react with the material constituting the organic material purification device 500 in the range where the degree of vacuum is not significantly lowered is used as an inert gas. The inert gas functions to flow the mixed sublimation gas 513 into the ionic liquid 541 in the storage tank 540, and mixes with the mixed sublimation gas 513 to form a mixed gas (S620).

The mixed gas 514 thus formed is mixed with the ionic liquid 541 through the connection duct 530 to form bubbles as the pressure inside the processing chamber 520 rises (S630). On the other hand, in the process in which the mixed gas 514 is mixed into the ionic liquid 541 through the connection duct 530, the second heater 531 provided around the connection duct 530 heats the periphery of the connection duct 530, thereby mixing the sublimation gas 513 to maintain sublimation. The state of the dots can be mixed into the ionic liquid 541.

On the other hand, the mixed gas mixed in the ionic liquid 541 forms a bubble, the mixed sublimation gas 513 in the bubble dissolves in the ionic liquid 541, the inert gas does not dissolve in the ionic liquid 541, and floats to the outside of the ionic liquid 541, and is collected in the storage tank 540. The upper part. The inert gas thus collected in the upper portion of the storage tank 540 is discharged to the outside of the storage tank 540 by the discharge pump 553 (S640). On the other hand, the inert gas discharged to the outside of the storage tank 540 is returned to the inert gas supply source 560 through the inert gas return means and can be recycled. Here, the inert gas retracting means is constituted by a general pump or the like.

When the mixed sublimation gas 513 is dissolved in the ionic liquid 541, since the content of the organic material of the purified article is absolutely higher than that of the impurity, the organic material first reaches a supersaturation state, and the recrystallization is first started to precipitate a high-purity purified material 543 (S650). At this time, the solubility of the mixed sublimation gas 513 dissolved in the ionic liquid 541 can be adjusted by the third heater 542 provided at the lower portion of the storage tank 540. Thereby, the solubility of the ionic liquid 541 mixed with the sublimation gas 513 is adjusted, and the ionic liquid 541 can control the supersaturation of the organic material, the recrystallization rate of the organic material, and the like. Therefore, the mixing of impurities can be minimized in the recrystallization process, so that the high-purity purification material 543 precipitated in the ionic liquid 541 can be appropriately recovered from the storage tank 540. For example, a port is formed on one side of the storage tank 540, and the purified material 543 is recovered.

As described above, after the high-purity purification material 543 precipitated in the ionic liquid 541 is recovered, a part of the ionic liquid 541 is contained before the organic material dissolved in the mixed gas and the small amount of impurities reach supersaturation. Further, as the purification procedure proceeds, the content of impurities in the ionic liquid 541 increases, and after a certain period of time, the impurity component also reaches a degree of supersaturation, and impurities are mixed in the recrystallized organic material. At this time, it is preferred to exchange the ionic liquid used for the purification process into a high-purity ionic liquid.

On the other hand, dissolved organic materials and impurities have different evaporation temperatures from ionic liquids. That is, the evaporation temperature of the ionic liquid is lower than that of the organic material and impurities. With this property, the ionic liquid components can be separated and purified separately. For this reason, when the third heater 542 is set to be heated at the evaporation temperature of the ionic liquid, the ionic liquid evaporates, and is collected in the collecting tank 572 through the collecting plate 571 of the ionic liquid collecting portion 570, leaving only the highly concentrated organic material and impurities. After the high-concentration organic materials and impurities remaining as described above are separately collected, the organic material and the impurities are separated by a re-treatment using a common solvent, and the organic material having a certain level of purity can be reused as a recrystallized raw material. In addition, the ionic liquid recovered in the collection tank 572 is returned to the inside of the storage tank 540 through the ionic liquid return means and can be recycled. Here, the ionic liquid retracting means is constituted by a general pump or the like.

On the other hand, in the organic material purification device 500 of the present embodiment, after the mixed gas is mixed into the ionic liquid 541 of the storage tank 540, the mixed sublimation gas 513 in the bubble is easily dissolved in contact with the ionic liquid 541, and the volume of the bubble may be included. A means of miniaturizing bubbles becomes smaller.

Further, the organic material purification device 500 of the present embodiment may further include a contact expansion means for allowing the mixed sublimation gas 513 to easily contact the ionic liquid 541. For example, in a state where the mixed sublimation gas 513 is mixed with the inert gas, it is guided to pass through the ionic liquid 541 for a certain period of time, whereby the dissolution of the sublimation gas can be promoted.

<Third embodiment>

Fig. 7 is a conceptual diagram showing the relationship of the constitution of an organic material purifying apparatus using an ionic liquid according to a third embodiment of the present invention. As shown in Fig. 7, the organic material purifying apparatus 500A according to the present embodiment is configured to enable the smooth recovery of the purified material 543A, except for partially changing the form of the storage tank 540A and the arrangement of the third heater 542A. The organic material purification device 500 of the embodiment has the same configuration. Therefore, the same component symbols are used for the same constituent elements in the present embodiment, and the description thereof will be omitted.

The storage tank 540A of the present embodiment has a lower portion formed in a funnel shape, and the lower side constitutes a recovery tank 544 having a purification material 543A alone. At this time, the recovery tank 544 is configured to be detachably coupled at the lower end of the storage tank 540A. Therefore, the purification material 543A precipitated through the above-described procedure is gradually accumulated in the recovery tank 544. On the other hand, a valve 545 for controlling the movement of the ionic liquid to the recovery tank 544 is also provided at a lower portion of the storage tank 540A. Therefore, when a certain amount of purified material 543A is accumulated inside the recovery tank 544, the valve 545 is closed. The purified material 543A is recovered by separating the recovery tank 544 from the storage tank 540A.

On the other hand, the third heater 542A of the present embodiment has a recovery tank 544 according to the lower portion of the storage tank 540A, and is heated in an indirect heating manner on the side surface of the storage tank 540A so that the purified material 543A can be smoothly deposited.

Hereinafter, the purification of the organic material using the ionic liquid as described above is included, and the purification effect will be described based on the experimental procedure, the results, and the like.

1. Simple purification experiment device for organic materials

Fig. 8 is a perspective view schematically showing the relationship between the constitution of an organic material simple purification experimental apparatus using an ionic liquid. As shown in Fig. 8, the organic material simple purification experimental device is mainly divided into a sublimation portion that sublimates the organic material raw material, a recrystallization portion that recrystallizes the organic material sublimation gas in the ionic liquid, and a recrystallized portion. Analytical section for analysis of organic materials (purified materials). On the other hand, the recrystallization unit and the analysis unit are composed of a ceramic heater, a thickness monitor, a thermo-couple, and a mask, and the sublimation unit is a shutter or a cymbal. And the heater is composed. The recrystallization unit is formed by applying an ionic liquid in the form of a droplet on the Si wafer, and then fixing it to the ceramic plate to be fixed to the ceramic heater. The sublimation unit is for loading the raw material of the purified material on the crucible.

In the experiment of the simple purification apparatus of the organic material constituted as described above, the evaporation amount of the organic material in the sublimation portion is controlled by the temperature of the sublimation portion, and the organic material supplied from the sublimation portion is crystallized in the ionic liquid. Adjusting the temperature of the ceramic heater explores the best crystallization temperature.

2. Organic material purification experiment preparation steps ( Sublimation Department )

The raw material of the organic material to be purified is weighed, put into the crucible, and placed inside the sublimation part. At this time, the organic material used is NPB (N, N'-di(biphenyl-4-yl)-N, N'-bis(2-methyl-biphenyl-4-yl)biphenyl-4, 4'-diamine ).

3. Organic material extraction experiment preparation steps ( Recrystallization Department and Analysis Department )

The ionic liquid was applied as a droplet on a Si wafer (50 x 50 mm ² ) and mounted on a shield. Then, after fixing the shield on the supporting member of the ceramic heater, the crystallization temperature of the organic material and the amount of the organic material supplied from the sublimation portion were confirmed by a thermocouple and a thickness measuring device, and the best organic material purification conditions were explored. . At this time, the ionic liquid used is OMIM TFSI.

4. Ceramic heater - Thermocouple temperature

Fig. 9 is a graph showing changes in substrate temperature in accordance with the set temperature of the ceramic heater in the organic material simple purification experimental apparatus shown in Fig. 8. It can be seen from Fig. 9 that after the set temperature of the ceramic heater installed in the experimental apparatus is raised to 300 to 500 ° C, the result of actually confirming the temperature of the recrystallization portion through the thermocouple is as shown in Fig. 9. Temperature gradient.

This temperature change experiment was performed to confirm that the crystallization temperature of the ionic liquid coated on the Si wafer was first performed. According to the experimental results, the actual crystallization temperature was not based on the temperature of the ceramic heater but the temperature measured by the thermocouple. A purification experiment was performed.

5. According to the deposition rate of sublimation temperature of organic materials in sublimation ( Crystallization temperature : R.T)

Fig. 10 is a graph showing the deposition rate and the change amount of the entire organic substance according to the sublimation temperature of the NPB organic material when the crystallization temperature (substrate temperature) is room temperature in the simple purification apparatus for organic materials shown in Fig. 8. In this experiment, the sublimation temperature of the sublimation part was changed when the crystallization temperature was room temperature, and the deposition rate and the entire thickness of the NPB organic material were analyzed by a thickness measuring device. The experimental results can be seen in Fig. 10, confirming that the sublimation temperature of the organic material increases, the deposition rate increases by 0.1 to 9 Å/sec, and the thickness of the whole organic substance changes from 0.011 to 1.64 μm.

6. According to the deposition rate of sublimation temperature of organic materials in sublimation ( Crystallization temperature : 100 °C )

Fig. 11 is a graph showing the deposition rate and the change amount of the entire organic substance according to the sublimation temperature of the NPB organic material when the crystallization temperature (substrate temperature) is 100 ° C in the simple purification apparatus for organic materials shown in Fig. 8. In this experiment, the sublimation temperature of the sublimation part was changed when the crystallization temperature was 100 ° C, and the deposition rate and the entire thickness of the NPB organic material were analyzed by a thickness measuring device. The experimental results can be seen in Fig. 11 to confirm that the higher the sublimation temperature of the organic material is, the deposition rate increases from 0.1 to 9.2 Å/sec, and the thickness of the entire organic material changes from 0.011 to 1.51 μm.

7. According to the deposition rate of sublimation temperature of organic materials in sublimation ( Crystallization temperature : 110 °C )

Fig. 12 is a graph showing the deposition rate and the change amount of the entire organic substance according to the sublimation temperature of the NPB organic material when the crystallization temperature (substrate temperature) is 110 ° C in the simple purification apparatus for organic materials shown in Fig. 8. In this experiment, the sublimation temperature of the sublimation part was changed at a crystallization temperature of 110 ° C, and the deposition rate and the entire thickness of the NPB organic material were analyzed by a thickness measuring device. The experimental results can be seen in Fig. 12, confirming that the sublimation temperature of the organic material increases, the deposition rate increases from 0.1 to 12.8 Å/sec, and the thickness of the entire organic substance changes from 0.013 to 2.37 μm.

8. In an ionic liquid through an optical microscope NPB Organic material crystallized image

Fig. 13 is a photograph showing the crystallization process of NPB organic material in an ionic liquid by an optical microscope according to the sublimation temperature of the organic material and the substrate temperature in the simple purification apparatus for organic materials shown in Fig. 8. As can be seen from Fig. 13, the sublimation temperature (180 ° C) of the sublimation portion did not cause sublimation of the NPB organic material, and no material was supplied to the ionic liquid. However, when the sublimation temperature of the NPB organic material is increased to 200 ° C or more, sublimation is started, and it is confirmed that the crystallization temperature (substrate temperature) of the ionic liquid increases, and the crystal grain size of the purified NPB organic material increases.

9. Through SEM Analytical ionic liquid NPB Organic material crystallized image

Fig. 14 is a NPB organic material crystallinity image (SEM analysis) manufactured by the simple purification apparatus for organic materials shown in Fig. 8. That is, Figure 14 is based on the results of crystallization analysis of NPB organic materials by optical microscopy, based on organic material sublimation temperature (200, 220 ° C), crystallization temperature (RT, 100, 110 ° C) versus NPB organic materials. The degree of crystallization was analyzed by SEM surface. As can be seen from Fig. 14, the crystallization temperature of the ionic liquid is RT. At 100 ° C, the crystallization degree of the NPB organic material shows the most outstanding characteristics, and the crystallization degree (110 ° C) shows that the degree of crystallization becomes low. phenomenon.

10. Through RAMAN analysis NPB Crystallographic phase analysis of organic materials

Fig. 15 is a graph showing the crystal phase of the NPB organic material recrystallized by the organic material simple purification experimental apparatus shown in Fig. 8 and the crystal phase of the NPB organic material before purification by Raman analysis. As can be seen from Fig. 15, the crystallization peak of the recrystallized NPB organic material shows 1125 under the purification conditions of the NPB organic material sublimation temperature (220 ° C) and crystallization temperature (substrate temperature) (110 ° C). The Raman shift value of 1199, 1222, 1289, 1328, 1375, 1529, 1574, 1609 cm ^-1 shows a Raman shift value almost identical to the crystalline phase of the NPB organic material before purification. This means that when recrystallization by the ionic liquid, the crystallinity of the raw material of the raw NPB is not lost and recrystallization is achieved.

11. Analyzed by optical microscope NPB Analysis of crystal size of organic materials

Figure 16 is a graph showing the crystal grain size (b) of the NPB organic material recrystallized by the simple purification apparatus for organic materials shown in Fig. 8 and the crystal grain size of the NPB organic material before purification (a) Photographs analyzed by optical microscopy . As can be seen from Fig. 16, the NPB organic material before purification is taken as an example, and the crystal grain shape and size are confirmed according to the magnification (x50, x100, x200), and the crystal grain shape of the random directional powder form is shown. The size also shows the particle size of multiple morphologies without a certain pattern. However, the NPB organic material recrystallized in an ionic liquid is taken as an example, and the crystal grain morphology having a dendrite structure is shown, and the maximum diameter of the crystallized NPB organic material is also 50 μm, thereby confirming the relative material substance. The crystallinity of NPB organic materials is greatly improved.

Raman data shows that the crystal phase of the raw material and the purified NPB organic material almost coincide, and it is difficult to accurately predict the improvement of the crystal phase. However, it is confirmed by optical microscopy that the ionic liquid purification method can maintain the crystal phase of the raw material. And increase crystallinity and crystal grain size.

12. in conclusion

The results of comparative analysis of the NPB organic material and the raw material purified by the ionic liquid confirmed the significant change of the recrystallized NPB organic material. Compared with the sublimation purification method for purifying organic materials through repeated iterative sublimation-condensation processes, the method of recrystallizing the supersaturation of the organic material in the ionic liquid is not only to simplify the procedure, but also to recrystallize only the pure organic material. It has the advantage of improving the purity.

On the other hand, although the experiment was carried out through a simple purification experimental apparatus for an organic material having a small capacity, it can be seen from the experimental results as described above that the simple purification technique and a large amount of purification techniques of the organic material like the present invention can be Be applicable.

Industrial utilization

Through the above examples and experimental examples, it can be seen that the present invention utilizes a purification procedure for the difference in solubility, in the process of repeated dissolution-recrystallization of organic substances and impurities in an ionic liquid, The organic material that achieves supersaturation is firstly recrystallized, and the purification and recrystallization of various organic materials can be performed by one procedure.

Further, the present invention purifies an organic material under a vacuum condition, thereby minimizing impurities supplied from an external pollution source, and obtaining a high-purity organic material (purified material).

In addition, since the present invention uses an ionic liquid as a screening program and performs a purification process in an ionic liquid, not only the carrier gas is not lost, but also the ionic liquid can be used after recovering the recrystallized organic material. The organic material is purified, thereby having the effect of saving raw material loss and manufacturing cost consumed in the purification process.

The technical matters of the organic material purification method and the purification apparatus using the ionic liquid of the present invention have been described above with reference to the accompanying drawings, but this is exemplified by a preferred embodiment of the present invention. Therefore, the present invention is not limited to the described embodiments, and it is obvious that those skilled in the art can implement various modifications and variations without departing from the spirit and scope of the invention. Modifications or modifications are intended to fall within the scope of the patent application of the present invention.

110‧‧‧Transparent substrate
120‧‧‧Anode
130‧‧‧ hole injection layer
140‧‧‧ hole transport layer
150‧‧‧Organic light-emitting layer
160‧‧‧Electronic transport layer
170‧‧‧Electronic injection layer
180‧‧‧ cathode
200‧‧‧ Sublimation purification unit
210‧‧‧2nd quartz glass tube
220‧‧‧1st quartz glass tube
230‧‧‧vacuum pump
240‧‧‧坩埚
250‧‧‧heater
260‧‧‧ Purified materials
300‧‧‧Simple material purification device
310‧‧‧Processing chamber
320‧‧‧坩埚
321‧‧‧Organic materials
322‧‧‧1st heater
330‧‧‧矽 substrate
331‧‧‧ ionic liquid
332‧‧‧2nd heater
333‧‧‧ Guard
334‧‧‧Support parts
335‧‧‧ thermocouple
340‧‧ ‧Shutter
350‧‧‧ Thickness measuring device
S410‧‧‧Step 410
S420‧‧‧Step 420
S430‧‧‧Step 430
S440‧‧‧Step 440
500‧‧‧Organic material purification unit
500A‧‧‧Organic material purification unit
510‧‧‧坩埚
511‧‧‧Organic materials
512‧‧‧1st heater
513‧‧‧ mixed sublimation gas
514‧‧‧ mixed gas
520‧‧‧Processing chamber
530‧‧‧Connecting catheter
531‧‧‧2nd heater
540‧‧‧ storage tank
540A‧‧‧ storage tank
541‧‧‧ ionic liquid
542‧‧‧3rd heater
542A‧‧‧3rd heater
543‧‧‧ Purified materials
543A‧‧‧ Purified materials
544‧‧‧Recycling bin
545‧‧‧ valve
550‧‧‧vacuum pump
551‧‧‧ Valve
552‧‧‧ Valve
553‧‧‧Draining pump
554‧‧‧ Valve
560‧‧‧Inert gas supply
570‧‧‧Ionic Liquid Collection Department
571‧‧‧ collecting board
572‧‧‧ collection bucket

Figure 1 is a conceptual diagram showing the structure of an OLED. Fig. 2 is a view schematically showing the configuration of a sublimation purification apparatus according to the prior art. Fig. 3 is a conceptual diagram showing the relationship of the constitution of an organic material simple purification apparatus using an ionic liquid according to the first embodiment of the present invention. Fig. 4 is a flow chart showing the purification method using the simple purification apparatus for an organic material using an ionic liquid shown in Fig. 3. Fig. 5 is a conceptual diagram showing the relationship of the constitution of an organic material purifying apparatus using an ionic liquid according to a second embodiment of the present invention. Fig. 6 is a flow chart showing the purification method using the organic material purifying apparatus using the ionic liquid shown in Fig. 5. Fig. 7 is a conceptual diagram showing the relationship of the constitution of an organic material purifying apparatus using an ionic liquid according to a third embodiment of the present invention. Fig. 8 is a perspective view schematically showing the relationship between the constitution of an organic material simple purification experimental apparatus using an ionic liquid. Fig. 9 is a graph showing changes in substrate temperature in accordance with the set temperature of the heater in the organic material simple purification experiment apparatus shown in Fig. 8. Fig. 10 to Fig. 12 are graphs showing the deposition rate and the change amount of the entire organic substance at each crystallization temperature (substrate temperature) in accordance with the sublimation temperature of the organic material in the simple purification apparatus for organic materials shown in Fig. 8. Fig. 13 is a photograph showing the crystallization process of the NPB organic material in the ionic liquid by optical microscopy according to the evaporation temperature of the organic material and the substrate temperature in the simple purification apparatus for organic materials shown in Fig. 8. Fig. 14 is a NPB organic material crystallinity image (SEM analysis) manufactured by the simple purification apparatus for organic materials shown in Fig. 8. Fig. 15 is a graph obtained by Raman analysis of the crystal phase of the NPB organic material recrystallized by the organic material simple purification experimental apparatus shown in Fig. 8 and the crystal phase of the NPB organic material before purification. Fig. 16 is a photograph of the crystal grain size of the NPB organic material recrystallized by the organic material simple purification experimental apparatus shown in Fig. 8 and the crystal grain size of the NPB organic material before purification by optical microscopy.

500‧‧‧Organic material purification unit

510‧‧‧坩埚

511‧‧‧Organic materials

512‧‧‧1st heater

513‧‧‧ mixed sublimation gas

514‧‧‧ mixed gas

520‧‧‧Processing chamber

530‧‧‧Connecting catheter

531‧‧‧2nd heater

540‧‧‧ storage tank

541‧‧‧ ionic liquid

542‧‧‧3rd heater

543‧‧‧ Purified materials

550‧‧‧vacuum pump

551‧‧‧ Valve

552‧‧‧ Valve

553‧‧‧Draining pump

554‧‧‧ Valve

560‧‧‧Inert gas supply

570‧‧‧Ionic Liquid Collection Department

571‧‧‧ collecting board

572‧‧‧ collection bucket

Claims (30)

A method for purifying an organic material using an ionic liquid, characterized in that the method for purifying an organic material of an OLED (Organic Light Emitting Diodes) by using an ionic liquid in a vacuum atmosphere comprises: a sublimation step of sublimating an OLED organic material containing impurities a step of dissolving the diffused gas of the organic material dissolved in the ionic liquid; and a recrystallization step of re-saturating the organic material in the ionic liquid, thereby recrystallizing the organic material. The method for simple purification of an organic material using an ionic liquid according to the first aspect of the invention is characterized in that, in the sublimation step, the organic material is sublimated by heating. The method for simple purification of an organic material using an ionic liquid according to claim 1, wherein the ionic liquid is coated on a substrate, and in the dissolving step, in order to adjust the solubility of the organic material Adjusting the temperature of the substrate. The method for simple purification of an organic material using an ionic liquid according to claim 3, wherein the temperature of the substrate is maintained in a range of from room temperature to 200 ° C in the dissolving step. An apparatus for simply purifying an organic material using an ionic liquid, characterized in that, as an apparatus for purifying an organic material of an OLED (Organic Light Emitting Diodes) by using an ionic liquid in a vacuum atmosphere, comprising: a sublimation means for sublimating an OLED organic material containing impurities; And a recrystallization means in which the sublimated gas of the diffused organic material is dissolved in the ionic liquid to supersaturate the organic material, thereby recrystallizing the organic material. The apparatus for simple purification of an organic material using an ionic liquid according to claim 5, wherein the sublimation means comprises: a crucible containing the organic material; and a treatment provided with the crucible and having a certain internal volume a cavity; a vacuum pump that evacuates the inside of the processing chamber; and a first heater that heats the crucible. The apparatus for simple purification of an organic material using an ionic liquid according to claim 6, wherein the sublimation means further comprises a shutter that selectively opens or closes an upper side of the crucible. The apparatus for simple purification of an organic material using an ionic liquid according to claim 6, wherein the recrystallization means comprises: a substrate coated with the ionic liquid; a shield supporting the substrate; a second heater that heats the substrate at an upper portion of the processing chamber; and a support member that supports the shield at a lower portion of the second heater. The apparatus for simple purification of an organic material using an ionic liquid according to claim 8, wherein the recrystallization means further includes a thermocouple provided on the support member to measure the temperature of the substrate, The temperature of the second heater is controlled by the temperature measured by the thermocouple. The apparatus for simple purification of an organic material using an ionic liquid according to the invention of claim 8, wherein the ionic liquid is applied to the substrate in the form of a droplet. The apparatus for simple purification of an organic material using an ionic liquid according to any one of claims 5 to 10, further comprising an analysis means for photographing and analyzing the recrystallized organic material. The apparatus for simple purification of an organic material using an ionic liquid according to claim 11, wherein the analysis means includes a thickness monitor for measuring a thickness of the recrystallized organic material. A method for purifying an organic material using an ionic liquid, characterized in that, as a purification method for purifying an OLED (Organic Light Emitting Diodes) organic material by using an ionic liquid in a vacuum atmosphere, comprising: a sublimation step of sublimating an OLED organic material containing impurities; a step of flowing a sublimation gas flowing the organic material into contact with the ionic liquid; a step of dissolving the sublimation gas in the ionic liquid; and supersaturating the organic material in the ionic liquid, thereby A recrystallization step of recrystallization of the material. The method for purifying an organic material using an ionic liquid according to claim 13 is characterized in that, in the flowing step, the sublimation gas is forcibly flowed by an inert gas into the ionic liquid stored in the storage tank. The method for purifying an organic material using an ionic liquid according to claim 14, wherein the dissolving step and the recrystallization step further comprise not dissolving and collecting in the upper portion of the storage tank. a step of discharging the inert gas to the outside of the storage tank. The method for purifying an organic material using an ionic liquid according to claim 13, wherein the recrystallization step further comprises a recovery step of recovering the recrystallized organic material from the ionic liquid. . The method for purifying an organic material using an ionic liquid according to claim 14, wherein the sublimation gas is maintained in a temperature above a sublimation point of the organic material before the sublimation gas is mixed into the ionic liquid. Heating step for gas heating. The method for purifying an organic material using an ionic liquid according to claim 13, wherein in the dissolving step, the temperature of the ionic liquid is adjusted in order to adjust the solubility of the organic material. The method for purifying an organic material using an ionic liquid according to claim 15, wherein the inert gas discharged in the discharging step is a carrier gas recovered as the flow step. An organic material purification device using an ionic liquid, characterized in that, as an apparatus for purifying an OLED (Organic Light Emitting Diodes) organic material by using an ionic liquid in a vacuum atmosphere, comprising: a sublimation means for sublimating an OLED organic material containing impurities; a means for flowing the sublimation gas of the organic material to contact the ionic liquid; and a recrystallization means for dissolving the sublimation gas in the ionic liquid to supersaturate the organic material, thereby recrystallizing the organic material . The apparatus for purifying an organic material using an ionic liquid according to claim 20, wherein the sublimation means comprises: a crucible containing the organic material; and a processing chamber provided with the crucible and having a certain internal volume; a vacuum pump that evacuates the interior of the processing chamber; and a first heater that heats the crucible. The apparatus for purifying an organic material using an ionic liquid according to claim 21, wherein the recrystallization means comprises: a storage tank for accommodating the ionic liquid; and one side and an inner portion of the processing chamber a connecting conduit that communicates with the ionic liquid immersed in the storage tank on the other side; and a vacuum pump that draws the inside of the storage tank into a vacuum state. The apparatus for purifying an organic material using an ionic liquid according to claim 22, further comprising a second heater for heating the outside of the connecting duct to maintain a sublimation point of the organic material. The apparatus for purifying an organic material using an ionic liquid according to claim 22, further comprising a third heating unit for heating the lower portion of the storage tank containing the ionic liquid in order to adjust the solubility of the organic material Heater. The apparatus for purifying an organic material using an ionic liquid according to claim 24, further comprising: disposed on an inner upper portion of the storage tank, the ionic liquid used in the purification of the organic material The liquid is collected by heating in a vacuum to a certain temperature or more and evaporated to collect the ionic liquid collecting portion. The apparatus for purifying an organic material using an ionic liquid according to claim 25, wherein the ionic liquid collecting portion comprises: a collecting plate fixed to an inner side surface of the storage tank; and being fixed in the storage tank A collecting bucket for collecting the ionic liquid collected by the collecting plate on the inner side. The apparatus for purifying an organic material using an ionic liquid according to claim 26, further comprising an ionic liquid retreating means for returning the ionic liquid collected by the collection tank to the storage tank. The apparatus for purifying an organic material using an ionic liquid according to claim 22, further comprising selectively communicating with the storage tank, and configured to be capable of combining and separating, and separately recovering the recrystallized organic Recycling bin for materials. The apparatus for purifying an organic material using an ionic liquid according to claim 22, wherein the flow means comprises an inert gas supply source for supplying an inert gas to a side of the processing chamber, the The crystallization means further includes a discharge pump that discharges the inert gas collected above the ionic liquid of the storage tank to the outside of the storage tank. The apparatus for purifying an organic material using an ionic liquid according to claim 29, further comprising an inert gas retracting means for returning the inert gas discharged through the discharge pump to the inert gas supply source.