KR20160043888A - Method for purifing vapor-phase organic materials and Apparatus for purifing vapor-phase organic materials - Google Patents

Abstract

An apparatus (1) for purifying a gas-phase organic material using an ionic liquid according to the present invention comprises a melting section (3) for melting a solid organic material containing an impurity, a vaporizing section And a collecting part (2) for collecting the vaporized gas by bringing the vaporized gas produced in the vaporizing part into contact with the flowing ionic liquid, wherein the collecting part collects the vaporized gas in the vaporized gas collected and dissolved in the ionic liquid The organic material to be refined is first supersaturated to produce a recrystallized organic material. The present invention can continuously supply the liquid organic material to the vaporizing part, so that it is not necessary to heat and cool the device for each predetermined amount of tablets as in the conventional sublimation purification device, and purification can be continuously performed . Therefore, the present invention can efficiently purify an organic material even if the amount of purification is increased.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for purifying vapor-phase organic materials using an ionic liquid,

The present invention relates to a purification method and apparatus for purifying an organic material using an ionic liquid, and more particularly, to an apparatus and a purification apparatus for purifying an organic material containing an impurity by an ionic liquid and purifying the organic material by recrystallization An organic material purification method and a purification apparatus.

BACKGROUND ART [0002] Conventional methods for purifying an organic material include solvent recrystallization, distillation, chromatography, sublimation purification and the like. Organic materials having high purity are used for organic light emitting devices (OLED) using organic materials. For this purpose, the most widely used purification method is a sublimation purification method. The sublimation purification method is a method which utilizes the difference in sublimation point of an organic material and forms a temperature gradient in the purification apparatus to separate and purify the target organic material and impurities. However, such a sublimation purification method has a limitation in the purification capacity per one time, and it is difficult to obtain a high purity organic material by only one purification, so that the purification process for the second and third steps is repeated. In addition, when the purification process is completed, the vacuum chamber is opened to the atmosphere, which is accompanied with the inconvenience of collecting the object organic matter in the solid phase. Such a sublimation purification method has a limitation in the yield of the high purity organic material, the working time, and the once-refined capacity.

To overcome these limitations, a sublimation device capable of high purity organic material purification by a continuous process and a refining device capable of increasing the purification capacity one time and allowing a continuous process have been devised. The purification apparatus described in Patent Document 1 (Korean Patent No. 10-1414160) has devised a method of dividing a purification section into two sections and performing a purification process twice in the same apparatus continuously to obtain a higher purity organic material. However, even in such a device, after the purification, the equipment is stopped to collect solid organic materials and the target organic material is collected while exposed to the atmosphere. At this time, there is a problem that the purity of the target organic material is lowered due to exposure to the impurities, and the refining process is interrupted, thereby limiting the refining capacity per unit time.

In Patent Document 2 (Korean Patent Laid-Open No. 10-2014-0079308), a sublimation gas of an organic material generated in a sublimation purification process of an organic material is mixed with a stable ionic liquid in a vacuum and supersaturated in an ionic liquid, A purification method capable of drastically improving the yield of purification of an organic material has been proposed. However, such a purification method using an ionic liquid has a problem in that a carrier gas is used in a process of continuously supplying a solid organic material to a vacuum chamber or mixing a sublimation gas of an organic material into an ionic liquid.

In Patent Document 3 (Korean Patent Laid-Open Publication No. 10-2014-0084165), an organic material to be refined is supplied as a liquid and vaporized. Then, the organic material and the impurities are separated in a liquid phase through a condensation process, By discharging it to the outside of the apparatus, it is possible to overcome the limit value of the once refining capacity possessed by the sublimation apparatus and to perform the purification process continuously without stopping the apparatus. However, fundamentally, the purification process in the above apparatus uses a principle of separation and purification of impurities using a condensation temperature difference (temperature gradient) similar to that of the sublimation purification apparatus. Therefore, there is a limitation in obtaining a high purity organic material by a one- Have. Therefore, in order to obtain a high-purity organic material in a one-time purification process, it is necessary to use a fundamentally different separation purification process.

Korean Patent No. 10-1414160 Korean Patent Publication No. 10-2014-0079308 Korean Patent Publication No. 10-2014-0084165

The present invention provides a method and apparatus for refining a gaseous organic material capable of recrystallizing a high purity organic material which is supersaturated by solubility difference after trapping and dissolving gaseous organic material containing impurities in an ionic liquid, There is a purpose.

Another object of the present invention is to provide a method and a device for purifying a gas-phase organic material capable of continuous purification by vaporizing a liquid organic material produced by melting a solid organic material and collecting it as an ionic liquid.

It is another object of the present invention to provide a purification method and purification apparatus for a vapor-phase organic material capable of continuously recovering recycled organic materials without interrupting the purification apparatus.

According to another aspect of the present invention, there is provided an apparatus for purifying a gas-phase organic material using an ionic liquid, comprising: a melting unit for melting a solid organic material containing impurities; And a collecting section for collecting the vaporizing gas by bringing the vaporizing gas generated by the vaporizing section into contact with an ionic liquid flowing in the vaporizing section, wherein the collecting section collects the vaporizing gas Characterized in that the organic material to be purified in the gas is first supersaturated to produce a recrystallized solid organic material.

According to the present invention, the collecting portion further comprises: a housing connected to communicate with the vaporizing portion; a plurality of blades disposed in the housing across a path through which the vaporizing body sprays; An ionic liquid supply means for supplying the ionic liquid, and a mixed liquid in which the vaporizable liquid is dissolved in the ionic liquid, and a storage means for storing the recrystallized organic material.

According to the present invention, there is further provided a circulation unit for circulating the mixed liquid from the storage unit along the surface of the plurality of blades.

According to the present invention, the collecting portion includes: a housing that communicates with the vaporizing portion; an ionic liquid supplying portion that supplies the ionic liquid so as to fall across a path in which the vaporizing body is scattered; And a storage means for storing the mixed liquid generated by dissolving the vaporizer body and the recrystallized organic material.

Further, according to the present invention, there is further provided a circulation unit for circulating the mixed liquid from the storage means and causing the vaporizer body to fall across a path through which the vaporizer is scattered.

In addition, according to the present invention, the circulation unit discharges the mixed liquid in the storage unit and the recrystallized solid organic material to the outside of the storage unit, separates and recovers the recrystallized solid organic material, And a recovery means for circulating the mixed liquid.

According to the present invention, the collecting portion includes: a housing connected to the vaporizing portion; at least one rotating roll disposed in the housing across a path through which the vaporizing body spans; And an ionic liquid storage portion for supplying the ionic liquid to the surface of the rotary roll.

According to the present invention, on one side of the rotary roll, a doctor blade is provided to peel the mixed liquid generated by dissolving the vaporizer in the ionic liquid from the surface of the rotary roll.

According to another aspect of the present invention, there is provided a method for purifying a gas-phase organic material using an ionic liquid, comprising the steps of: melting a solid organic material containing an impurity; A step of collecting the vaporized gas by bringing the vaporized gas of the organic material into contact with an ionic liquid flowing in the vaporized gas to vaporize the organic material to be purified, And a recrystallization step of first producing a recrystallized solid organic material by supersaturation.

Further, according to the present invention, in the collecting step, the ionic liquid flows along the surface of the plurality of blades disposed across the path of scattering of the vaporizer body.

According to the present invention, the recrystallization step further comprises a circulation step of circulating the mixed liquid generated by dissolving the vaporizer in the ionic liquid along the surfaces of the plurality of blades.

Further, according to the present invention, in the collecting step, the ionic liquid flows downward across a path through which the vaporizer body is scattered.

Further, according to the present invention, in the recrystallization step, a circulation step of circulating the mixture liquid generated by dissolving the vaporizer body in the ionic liquid across the path of scattering the vaporizer body is further included.

According to the present invention, in the circulation step, the recrystallized solid organic material is filtered and the mixed liquid is circulated.

According to the present invention, in the collecting step, the ionic liquid is applied and flows on the surface of at least one rotary roll disposed across the path of scattering of the vaporizer body.

According to the present invention, there is further provided a step of peeling off the mixed liquid generated by dissolving the vaporizer in the ionic liquid using the doctor blade from the surface of the rotating roll.

The present invention can continuously supply the liquid organic material to the vaporizing part, so that it is not necessary to heat and cool the device for each predetermined amount of tablets as in the conventional sublimation purification device, and purification can be continuously performed . Therefore, according to the present invention, it is possible to efficiently purify an organic material even if the purification amount is increased.

The purification separation process used in this invention uses a process in which the organic material is recrystallized in the ionic liquid by a concentration gradient of the organic material for the OLED in the ionic liquid rather than by a temperature gradient so that a more thermodynamic equilibrium state The target organic material and the impurities are purified. Therefore, the recrystallization by the concentration gradient causes the organic material as the main stream to reach the supersaturation first and then recrystallize. Therefore, it is possible to accurately separate the impurities and the organic material in the ionic liquid. Therefore, Can be purified.

1 is a schematic block diagram of an apparatus for purifying a vapor organic material according to the present invention,
2 is a schematic view of an apparatus for purifying a gas phase organic material according to a preferred embodiment of the present invention,
3 is a schematic view of the melting portion shown in Fig. 2,
Fig. 4 is a schematic view of the vaporization portion shown in Fig. 2,
5 is a schematic view for explaining the concept of the circulation unit shown in Fig. 2,
Figs. 6 to 11 are views showing various modifications of the collecting portion shown in Fig. 2, respectively, Figs. 6 to 8 show various vertical blade structures respectively, and Fig. 9 shows a horizontal blade structure Fig. 10 shows a spray-type structure, Fig. 11 shows a rotary-roll structure,
12 is a flowchart of a method for purifying a vapor organic material according to the present invention.

Best Mode for Carrying Out the Invention Hereinafter, preferred embodiments of a method and apparatus for purifying a gas-phase organic material using an ionic liquid according to the present invention will be described in detail with reference to the accompanying drawings.

(1) Composition of the purification apparatus

1 is a schematic view of an apparatus 1 for purifying a vapor organic material according to the present invention. 1, the refining apparatus of the present invention comprises heating a solid organic material S1 to produce a liquid organic material L1, vaporizing the organic material L1 in the liquid phase, And the vaporized gas V1 of the organic material supplied from the vaporizing unit is collected and dissolved in ionic liquids (ILs) L2 to produce a mixed liquid L3 and a solid The organic material S2 is obtained and the mixture L3 + S2 is circulated to separate the solid organic material S2 and the remaining mixture L3 is used to collect the vaporized organic material V1.

FIG. 2 is a schematic view of an apparatus for purifying a gas phase organic material according to a preferred embodiment of the present invention. 1 and 2, the refining apparatus 1 comprises a melting unit 3 for melting a solid organic material S1 containing an impurity to produce a liquid organic material L1, A vaporizing portion 6 for vaporizing the liquid organic material L1 supplied from the vaporizing portion 6 to generate a vaporizing gas V1 of an organic material and a vaporizing portion 6 for vaporizing the organic material supplied from the vaporizing portion 6 (2) for collecting and dissolving the vaporizing gas (V1) in the ionic liquid (L2) by contacting the flowing ionic liquid (L2) with the ionizing liquid (V1) And a circulation unit 4 for separating the solid organic material S2 and circulating the remaining mixed liquid L3 to the collecting unit 2 by receiving the mixed liquid L3 + L3. On the other hand, in the collecting part 2, the organic material to be refined, which is the main component of the composition, among the vaporized gas V1 which is captured and dissolved in the ionic liquid L2 is first supersized to produce a recrystallized solid organic material S2 . An ionic liquid supply part 7 for supplying the ionic liquid L1 is connected to one side of the collecting part 2. [

(1-1)

As shown in FIG. 2, the melting unit 3 melts and melts a solid organic material for OLED S1, and continuously supplies a liquid organic material into the vaporizing unit 6. As shown in FIG. The solid organic material S1 as a starting material contains 0.1 to 10 wt%, preferably 0.1 to 5 wt%, and most preferably 0.1 to 2 wt% of impurities. On the other hand, it is preferable that such an organic material has a melting point (Tm) which is melted by heating under a temperature range in which the organic material is thermally decomposed and not denatured. As an organic material raw material according to this embodiment, NPB (naphthylen-1-yl) -N, N'-bis (phenyl) -benzidine) material used as a hole transport layer (HTL) have.

On the other hand, there are various organic material raw materials used for manufacturing OLED devices in addition to the above materials. Therefore, the present invention can use various kinds of organic materials that can be melted as a raw material.

The melting unit 3 includes a raw material replenishing unit 3A for melting a solid organic material and a supplying unit 3B formed on the discharging side of the melting tank 31 to store the liquid organic material and supply it to the vaporizing unit 6. [ And supply amount control means 3C formed on the discharge side of the supply tank 32 for controlling the supply amount to the vaporization portion 6. [

In the present invention, the term " continuously supplying " means not only continuously supplying the organic material but also continuously supplying and stopping the organic material by a predetermined period or a different period in a state in which the purification apparatus is continuously operated without stopping And in this embodiment, supply and stop of the material for OLED is controlled by the supply amount control means 3C.

end. The raw material supply device (3A)

3 is a schematic view of the melting portion shown in Fig. As shown in FIGS. 2 and 3, the raw material supply device 3A includes a hopper 34 for supplying a solid organic material for an OLED, and a hopper 34 for supplying a solid organic material for OLED and a molten organic material for OLED A vacuum pump 36a for reducing the pressure of the interior of the fusion tank 31 and an infrared heater 35 for heating the fusion tank 31. [

The fusion tank 31 is constituted by a pressure-resistant container, and the solid organic material for OLED is fused in the fusion tank 31. The fusion tank 31 is preferably made of a material inert to the OLED organic material, and in this embodiment is made of quartz glass.

The hopper 34 is connected to the fusion tank 31 by a pipe member D1 and a valve 31a is formed in the middle of the pipe member. Feeding of the solid organic material for OLED from the hopper 34 into the fusion tank 31 is controlled by opening and closing the valve 31a. The hopper 34 is preferably made of a material inert to the OLED organic material, and in this embodiment is made of quartz glass. Further, in this embodiment, the lid 34a is mounted on the upper portion of the hopper 34 so as to be openable and closable, thereby preventing the solid organic material for OLED from deteriorating due to light deterioration or contact with the air.

The vacuum pump 36a is connected to the fusion tank 31 by a piping member, and a valve 31c is formed in the middle of the piping member. In this embodiment, the pressure in the fusion tank 31 is 10 ^-1 Pa or less. Further, the inside of the fusion tank 31 may be evacuated by the vacuum pump 36a, and then filled with nitrogen.

The infrared heater 35 is disposed so as to surround the outer periphery of the fusion tank 31. Further, the infrared heater 35 is connected to the temperature controller 8. The infrared heater 35 heats the fusion tank 31 such that the solid organic material for OLED supplied into the fusion tank 31 is melted. Specifically, the inside of the fusion tank 31 is heated up to the melting point of the organic material for OLED to be fused.

The temperature of the melting tank 31 heated by the infrared heater 35 is measured by a temperature sensor (not shown) connected to the temperature controller 8. The measured temperature information is transmitted to the temperature controller 8, and the temperature controller 8 controls the heating by the infrared heater 35 based on the received temperature information.

I. The supply part (3B)

2 and 3, the supply unit 3B includes a supply tank 32 for temporarily storing the liquid organic OLED material until the vaporized portion 6 is supplied to the vaporization unit 6, An infrared heater 37 for heating the supply tank 32 and a storage amount control means 36 for detecting and controlling the amount of liquid organic OLED material stored in the supply tank 32, (38).

The supply tank 32 is disposed on the discharge side of the fusion tank 31. The supply tank 32 is constituted by a pressure-resistant container. The supply tank 32 is preferably made of a material inert to the OLED organic material, and in this embodiment is made of quartz glass.

The discharge side of the fusion tank 31 and the inlet side of the supply tank 32 are connected by a pipe member D2. A valve 31b is formed in the middle of the pipe member D2. The valve 31b controls the supply of the liquid organic OLED material from the fusion tank 31 to the supply tank 32. [ In this embodiment, the supply tank 32 is provided at a position lower than the melting tank 31. Therefore, when the valve 31b is opened, the liquid organic OLED material can be moved into the supply tank 32 by its own weight.

A piping member D3 is connected to the discharge side of the supply tank 32. [ 2 or 4, the piping member D3 is inserted into the vaporizing section 6 and its tip is connected to the nozzle 64 above the inside of the vaporizing section 6. As shown in Fig.

A heater (not shown) is disposed on the outer periphery of the piping members D2 and D3. Therefore, solidification of the OLED organic material in the piping members D2 and D3 can be prevented.

The vacuum pump 36b is connected to the supply tank 32 by a piping member, and a valve 32a is formed in the middle of the piping member. In this embodiment, the pressure in the supply tank 32 is 10 ^-1 Pa or less. Further, the inside of the supply tank 32 may be evacuated by the vacuum pump 36b, and then nitrogen may be charged.

The infrared heater 37 is disposed so as to surround the outer circumference of the supply tank 32. Further, the infrared heater 37 is connected to the temperature controller 8. The infrared heater 37 heats the supply tank 32 so that the organic material for OLED contained in the supply tank 32 becomes a temperature at which the organic material does not solidify. Specifically, the inside of the supply tank 32 is heated up to the melting point of the organic material for OLED to be fused. The organic material for OLED supplied from the fusion tank 31 while remaining unmelted can also be melted in the supply tank 32.

The temperature of the supply tank 32 heated by the infrared heater 37 is measured by a temperature sensor (not shown) connected to the temperature controller 8. The measured temperature information is transmitted to the temperature controller 8, and the temperature controller 8 controls the heating by the infrared heater 37 based on the received temperature information.

The storage amount control means 38 controls the liquid level of the liquid organic OLED material in the supply tank 32 and the stored amount based on the information detected by the liquid level detection sensor 38a And a storage controller 38b for controlling the storage controller 38b. The information detected by the liquid level detection sensor 38a is transmitted to the storage amount controller 38b.

The liquid level detecting sensor 38a of this embodiment is composed of three temperature sensors 381a, 382a, and 383a. 3, a temperature sensor 381a is disposed below the supply tank 32, a temperature sensor 382a is disposed between the temperature sensor 381a and the temperature sensor 383a, and a temperature sensor 383a is disposed above the temperature sensor 382a .

The storage controller 38b receives the temperature information detected by the liquid level detection sensor 38a and determines the storage amount of the liquid organic OLED material in the supply tank 32 based on the temperature information. As shown in Fig. 3, in this embodiment, the temperature detected by the temperature sensor 383a located above the liquid level and the temperature detected by the temperature sensors 381a and 382a located below the liquid level are different. The storage controller 38b determines the liquid level and the storage amount based on different values of the detection temperatures. The storage controller 38b displays the determination result of the storage amount on the display means 38c composed of a display or the like. When the storage controller 38b determines that the liquid organic OLED material necessary for continuous refining is not stored in the supply tank 32, it displays this on the display means 38c, You can also make a sound. The operator can determine whether to add the organic material for OLED to the fusion tank 31 and to supplement the supply tank 32 based on the indication or the alarm sound.

Alternatively, the storage controller 38b may be connected to the temperature controller 8, the vacuum pumps 36a and 36b, and the valves 31a, 31b, 31c, and 32a so as to include the storage controller 38b. The storage controller 38b may be configured to control their operation and to automatically perform additional replenishment to the supply tank 32. [

All. The supply amount control means 3C

The supply amount control means 3C is disposed on the discharge side of the supply tank 32 and controls the amount of liquid organic material for OLED to be supplied to the vaporizing portion 6. [ 2 and 4 show supply amount control means 3C. 4 is a schematic view for explaining the concept of the vaporizing portion shown in Fig.

2 and 4, the supply amount control means 3C includes a supply pump 33 formed in the middle of the pipe member D3 connected to the discharge side of the supply tank 32, A valve 33a formed between the supply pump 33 and the supply pump 33 and a valve 33b formed between the supply pump 33 and the vaporization unit 6 and a liquid level detection sensor (39a) and a valve controller (39b) connected to the liquid level detection sensor (39a).

The supply pump 33 and the valves 33a and 33b control the supply amount of the liquid organic OLED material discharged from the supply tank 32 and supplied to the vaporizing part 6. [ When the liquid organic OLED material in the supply tank 32 is supplied into the vaporizing portion 6 by its own weight, the supply amount control means 3C does not need to include the supply pump 33. [

The liquid level detecting sensor 39a detects the remaining amount of the liquid organic material remaining in the container 63. In this embodiment, the liquid level detecting sensor 39a detects the liquid level in the container 63. [ The information detected by the liquid level detection sensor 39a is transmitted to the valve controller 39b.

The liquid level detection sensor 39a is composed of three temperature sensors 391a, 392a, and 393a in the same manner as the liquid level detection sensor 38a described above. 4, a temperature sensor 391a is disposed at a lower portion in the depth direction of the container 63, a temperature sensor 392a is disposed at an intermediate portion thereof, and a temperature sensor 393a is disposed at an upper portion thereof .

The valve controller 39b receives the temperature information detected by the liquid level detection sensor 39a and determines the level and level of the liquid level of the liquid organic material in the container 63 based on the temperature information. As shown in Fig. 4, in this embodiment, the temperature detected by the temperature sensor 393a located above the liquid level and the temperature detected by the temperature sensors 391a and 392a located below the liquid level are different. The valve controller 39b judges the remaining amount based on a different value of the detected temperature. The valve controller 39b is connected to the display means 39c constituted by a display or the like, and can display the result of determination of the remaining amount on the display means 39c.

The valve controller 39b is also connected to the supply pump 33 and the valve 33b so that the supply pump 33 and the valve 33b are closed so that the remaining amount of the liquid organic material in the container 63 is within a predetermined amount. . In this manner, the valve controller 39b automatically controls the supply of the liquid organic material to the vaporizing portion 6. [

(1-2)

As shown in Figs. 2 and 4, the vaporizing section 6 is connected to the melting section 3 on the upstream side of the purification system and communicates with the collecting section 2 on the downstream side. The vaporizing section 6 includes a hollow body 61, a heater 62 disposed outside the hollow body 61, and a receiving container 63 disposed inside the hollow body 61.

The inside of the hollow body 61 is subjected to a decompression process before the liquid organic material is supplied. At the substantially central portion of the inside of the hollow body 61, a storage container 63 for storing a liquid organic material for OLED is disposed.

For example, the accommodation container 63 is formed in a plate shape having a bottom surface in a rectangular plate shape and a side surface rising in the out-of-plane direction from the peripheral edge of the bottom surface. A nozzle 64 is disposed above the storage container 63 so as to direct the discharge port to the storage container 63. The nozzle 64 discharges the liquid organic OLED material supplied from the fusing unit 3 toward the inside of the receptacle 63 on the dish. The heating heater 62 is constituted by a heating wire heater or the like and annularly arranged on the outside of the hollow body 61.

The temperature controller 8 includes a temperature sensor 81 for measuring the temperature inside the vaporizing section 6, a temperature sensor 82 for measuring the temperature inside the collecting section 2, and temperature sensors 81 and 82 And a control unit 83 for controlling the heating heater 62 and the heating heater 22 based on the measured temperature information.

The temperature sensor 81 is disposed inside the hollow body 61 and the temperature sensor 82 is disposed inside the housing 21 and connected to the control unit 83 disposed outside the hollow body. The temperature information measured by the temperature sensors 81 and 82 is sent to the control unit 83. [ On the other hand, although only one temperature sensor 82 is shown in Fig. 2, it may actually be disposed corresponding to the inlet side, intermediate side, and outlet side positions of the respective collecting units 2. [ The temperature sensors 81 and 82 are not particularly limited, but a thermocouple is used in this embodiment.

The control unit 83 is connected to the heating heater 62 and the heating heater 22 and controls the heating of the heating heater 62 and the heating heater 22 based on the temperature information input from the temperature sensors 81 and 82 . In this embodiment, the control unit 83 can separate the sections of the collecting unit 2 and independently control the heater 22 for each section. For example, the control unit 83 controls the heating heater 22 so that the mixed liquid is continuously or stepwise different so as to maintain the same temperature for each section. The temperature of the mixed liquid is maintained as high as possible to promote dissolution of the vaporized gas captured in the ionic liquid.

The material of the hollow body 61 and the container 63 is preferably made of a material inert to the OLED organic material, and this embodiment is made of quartz glass.

(1-3) Ionic Liquid Supply Unit

2, the ionic liquid supply unit 7 includes a supply tank 71 for storing an ionic liquid used as a solvent for trapping and dissolving a vaporized organic material in the trapping unit 2, And a heating heater 72 for heating the supply tank 71. A vacuum pump 73 is connected to the supply tank 71 by a piping member, and a valve 73a is formed in the middle of the piping member. In this embodiment, the pressure in the supply tank 71 is 10 ^-1 Pa or less. The ionic liquid is decompressed through the vacuum pump 73 and stored in the supply tank 71 and is temporarily supplied to the collecting part 2 through the regulating valve 74 when a new solvent is required in the collecting part 2 . The supply temperature of the ionic liquid is preferably supplied in a heated state so as to have a temperature suitable for trapping and dissolving the vaporized gas of the organic material. The supply amount of the ionic liquid is determined according to the design capacity of the collector 2.

The ionic liquid according to this embodiment is used for purifying and recrystallizing an organic material and has a temperature range of 40 to 400 ° C, preferably 100 to 120 ° C, and a temperature of 10 ^-1 torr or less, preferably 10 ^-7 torr, it can be used as a solvent in a vacuum process.

As the ionic liquid used in this example, 1-butyl-3-methylimidazorium bis (trifluoromethyl sulfonyl) imide (1-butyl-3-methylimidazolium) imide BMIM TFSI) or 1-octyl-3-methylimidazorium bis (trifluoromethylsulfonyl) imide (OMIM TFSI) of formula (2) Can be used. Alternatively, 1-ethyl-3-methylimidazorium bis (trifluoromethylsulfonyl) imide (EMIM TFSI) may be used.

The above ionic liquids (BMIM TFSI, OMIM TFSI, and EMIM TFSI) are non-volatile organic solvents, which are organic materials and impurities which dissolve in the ionic liquid and which reach the supersaturation more rapidly Due to the mechanism that the material first recrystallizes, it can be used to purify and recrystallize various organic materials.

On the other hand, BMIM TFSI, OMIM TFSI and EMIM TFSI are low melting point, low vapor pressure, nonflammable, consist of organic molecular ions, And controllable properties by combinations of anions and cations.

(1-4) Collection section

The collecting section 2 is a device for collecting and dissolving a vaporized gas of an organic material supplied from the vaporizing section 6 via the valve 65 into an ionic liquid. Here, the collecting section 2 includes a housing 21, a heating heater 22 for supplying heat necessary for keeping the inside of the housing 21 at a temperature suitable for dissolving the organic vaporizer in the ionic liquid And flow means for causing the ionic liquid to flow to collect the vaporized gas of the organic material. Such a flow means may be provided with a movable structure such as a rotating screw (blade), a spray, a rotating roll, or a fixed structure that flows by the weight of the ionic liquid. In this embodiment, the fixed structure shown in FIGS. 2 and 5 can be used. The fixed structure is composed of a plurality of grid plates 25 disposed on the upper and lower sides of the inner wall of the housing 21 so as to be staggered left and right.

The movable structure may be constituted by the components described in Korean Patent Application No. 2015-0012661 filed by the inventor of the present invention.

Figs. 6 to 11 are views showing various modifications of the collecting portion shown in Fig. 2, respectively, Figs. 6 to 8 show various vertical blade structures respectively, and Fig. 9 shows a horizontal blade structure FIG. 10 shows a spray-type structure, and FIG. 11 shows a rotary-roll structure.

As shown in Figs. 6 to 9, the collecting units 2A, 2B, 2C, and 2D include housings 21A, 21B, 21C, and 21D connected to communicate with the vaporizing unit 6 25B, 25C, and 25D and the plurality of blades 25A, 25B, 25C, and 25D disposed in the housings 21A, 21B, 21C, and 21D across the scattering path (Such as the valve 74 in Fig. 2) for supplying the ionic liquid, and a storage means 26A, 26B, 26C for storing the mixed liquid and the recrystallized organic material in which the vaporizer body is dissolved in the ionic liquid, 26C, and 26D. On the other hand, the mixed liquid can be circulated along the surfaces of the plurality of blades 25A, 25B, 25C and 25D from the storage means 26A, 26B, 26C and 26D by the circulating unit 4 shown in Fig.

As shown in Figs. 6 to 8, the plurality of blades 25A, 25B, and 25C are arranged to rotate at equal angles about a vertical axis in the housings 21A, 21B, and 21C. 6, the blades 25A, 25B, and 25C may be provided in the form of a screw along the circumferential surface of the hollow shaft as shown in FIG. 6, or may be formed in the shape of a hollow shaft extending from one end to the other end along the circumferential surface of the hollow shaft, The phase difference may be set to have a turning angle of, for example, about 120 DEG, or may be equally spaced along the circumferential surface in the longitudinal direction of the hollow shaft as shown in FIG. On the other hand, the ionic liquid is supplied to the blade 25A (25A) through a plurality of injection pipes 27C which flow along the inside of the shaft of the hollow shape and spray on the surface of the blade 25C or the hole communicating with the surfaces of the blades 25A and 25B , 25B, 25C.

As shown in Fig. 9, the plurality of blades 25D are arranged to rotate at an equal angle about a horizontal axis in the housing 21D.

10, the collecting section 2E includes a housing 21E that communicates with the vaporizing section 6 (see FIG. 2), and an ionic liquid supplying section 22E for supplying the ionic liquid so as to fall across the path in which the vaporizing body is scattered. A liquid supply means (such as the valve 74 and the plurality of injection pipes 25E in Fig. 2), and a storage means 26E for storing the mixed liquid produced by dissolving the vaporizer in the ionic liquid and the recrystallized organic material . Here, the plurality of injection pipes 25E each have a plurality of nozzles for spraying the ionic liquid. On the other hand, the mixed liquid can be circulated by the circulating unit 4 shown in Fig. 2 so as to fall from the storage means 26E across the path in which the vaporizer body spans.

The circulation unit 4 discharges the mixed liquid in the storage means and the recrystallized solid organic material to the outside of the storage means as described later and then filters the recrystallized solid organic material and mixes the mixed liquid into the storage means Respectively.

11, the collecting portion 2F includes a housing 21F communicating with the vaporizing portion 6 (see Fig. 2), and a plurality of rotors 21C disposed in the housing 21F across the path in which the vaporizing body sprays. A roll 25F and an ionic liquid storage 26F disposed below the rotary roll 25F to supply the ionic liquid to the surface of the rotary roll 25F. On the other hand, on one side of the rotary roll 25F, a doctor blade 27F for dissolving the vaporizer in the ionic liquid and stripping the resulting mixed liquid from the surface of the rotary roll 25F may be further provided.

(1-5)

5 is a schematic diagram illustrating the concept of the circulation unit shown in Fig. 2 and 5, the circulation unit 4 is connected to the discharge valve 44 whose upstream side is formed at the bottom of the collection unit 2 and whose downstream side is connected to the circulation And is connected to the valve 46. The circulation unit 4 includes a discharge valve 44 for controlling the discharge amount of the mixed liquid discharged from the collecting unit 2, a transfer pump 42 for transferring the discharged mixed liquid through the valves 42a and 41a, A circulation pump 41 for circulating the mixture liquid separated from the recovery container 41 through the intermediate valves 41c and 45a to the inside of the collector 2, And a circulation valve 46 for regulating the amount of the mixed liquid circulated into the collecting part 2. The recovery vessel 41 includes an element (not shown) for separating the recrystallized organic material from the mixed liquid by filtration, centrifugal separation, or the like. Here, the recovery vessel 41, the circulation pump 45, the circulation valve 46, etc. discharge the mixed liquid and the recycled solid organic material to the outside of the collecting unit 2 and then remove the recrystallized organic material And serves as a recovery means for circulating the mixed liquid.

The discharge valve 44 is connected to the bottom of the collecting part 2. The discharge valve 44 and the recovery container 41 are connected by a pipe member D4. A feed pump 42, a valve 42a and a valve 41a are formed in this order from the discharge valve 44 side in the middle of the pipe member D4. The recovery container 41 and the vacuum pump 43 are connected by a piping member, and a valve 41b is formed in the middle of the piping member.

The transfer pump 42 and the valves 44 and 42a control the discharge amount of the mixture (mixed liquid and solid organic material) discharged from the collecting part 2 to the recovery container 41. [ When the mixture in the collecting device 2 is discharged into the recovery container 41 by its own weight, the transfer pump 42 may not be provided.

The circulation valve (46) is connected to one side of the collecting part (2). The circulation valve 46 and the recovery container 41 are connected by a piping member D5. A circulation pump 45, a valve 45a and a valve 41c are formed in this order from the side of the circulation valve 46 in the middle of the piping member D5.

In this embodiment, the pressure in the recovery container 41 is 10 ^-1 Pa or less. In addition, the purified solid organic material for OLED may be recovered after circulation in the state of being filled with nitrogen in the recovery container 41. The recovery container 41 is detachably formed between the valve 41a and the valve 42a, between the valve 41c and the valve 45a, and between the valve 41b and the vacuum pump 43 . Therefore, the recovery container 41 can be separated from the circulation unit 4 in a state in which the recovery container 41 is closed for replacement after the end of the circulation. After the separation, an empty recovery container 41 prepared separately can be mounted.

Since the recovery container 41 stores the recycled organic material for OLED in the inside thereof, it is preferable that the recovery container 41 is made of a material inert to the organic material for OLED. The transfer pump 42 is connected between the discharge valve 44 and the valve 42a and transfers the discharged mixture to the recovery container 41. [

A heating heater (not shown) is also disposed on the outer periphery of the pipe member D4, so that further recrystallization due to a temperature difference can be prevented in the course of feeding the mixture in the pipe member D4. Likewise, a heating heater (not shown) is also disposed on the outer periphery of the pipe member D5 so that the mixed liquid in the pipe member D5 circulates in the liquid collector into the collector 2 without further recrystallization due to a temperature difference in the circulation process .

The solid organic material separated in the recovery container 41 by filtration or the like is isolated or stored in an appropriate space inside the recovery container 41. [ On the other hand, the circulation to the inside of the trapping device 2 continues until the impurities are recrystallized in the mixed liquid inside the trapping device 2. Recrystallization of the impurities is detected by appropriate monitoring of recrystallized organic material in the mixed liquor inside the collector 2.

On the other hand, when the recrystallization of the impurities is detected in the collector 2, the supply of the liquid organic material is stopped, and the purified, purified organic material isolated in the recovery container 41 is collected, 4) is collected in the recovery container 41 and reprocessed.

(1-6) Organic materials for OLED

The organic material for OLED for purification is not particularly limited as a material used for the organic EL device. Among them, known materials useful for purifying by the purification apparatus of the present invention include, for example, N, N'-di- (naphthalen-1-yl) -N, N'-diphenyl-benzidine (NPB) .

(2) Purification method using a purification apparatus

Next, a method of purifying the organic material for OLED using the purification apparatus 1 will be described. 12 is a flowchart of a method for purifying a vapor organic material according to the present invention.

12, the method for purifying a vapor organic material according to the present invention comprises a melting step (S110) for melting a solid organic material containing an impurity, a liquid phase organic material produced in the melting step (S110) A vaporizing step (S120) of vaporizing the organic material; a collecting step (S130) of collecting the vaporizing gas by bringing the vaporizing gas of the organic material into contact with the flowing ionic liquid; and a collecting step And a recrystallization step (S140) of forming a recrystallized organic material by first supersaturation of the organic material.

(2-1) A process of melting a solid organic material for OLED (melting step (S110))

As shown in Fig. 3, the organic material for solid OLED for the pre-purification is supplied to the hopper 34 first. Next, the valve 31a is opened with the valve 31c closed, and a predetermined amount of solid organic material for OLED is supplied into the fusion tank 31. Then, After the supply, the valve 31a is closed, the valve 31c is opened, and the pressure in the fusion tank 31 is reduced to 10 ^-1 Pa or less with the vacuum pump 36a.

After the pressure reduction, the melting tank 31 is heated by the infrared heater 35 to melt the solid organic material for OLED. The heating by the infrared heater 35 is controlled by the temperature controller 8.

The molten organic material for the OLED in the melting tank 31 is decompressed in the supply tank 32 and the supply tank 32 is heated by the IR heater 37 for the OLED The organic material is heated to a temperature at which the organic material does not solidify, and the liquid organic OLED material is prepared. The valve 31a is opened with the valve 33a closed so as to supply the organic material for liquid OLED into the supply tank 32. [ After the supply, the valve 31b is closed and heating by the infrared heater 35 is stopped.

(2-2) A step of vaporizing the liquid organic OLED organic material in the vaporizing part (vaporization step (S120))

The process of vaporizing the liquid organic OLED organic material in the vaporization unit 6 of the purification system is as follows.

After the above-mentioned melting step or during the melting step, preparation of the organic material for OLED is carried out as follows. First, while the discharge valve 44 and the valve 33b are closed, the inside of the housing 21 is decompressed to 10 ^-1 Pa or less by the vacuum pump 23. After the pressure is reduced, the hollow body 61 of the vaporizing part 6 is heated by the heating heater 62, and the housing 21 of the collecting part 2 is heated by the heating heater 22. At this time, the temperature controller 8 controls the heating by the heating heater 62 and the heating heater 22 based on the measured temperature information of the temperature sensors 81 and 82. Specifically, the heating heater 62 heats the hollow body 61 to a temperature at which the liquid organic material evaporates (evaporation temperature), and maintains the temperature. Further, the heating heater 22 independently heats the collecting part 2 to a predetermined temperature. In this embodiment, the temperature (trapping temperature) of the trapping portion where the vaporizer body of the organic material to be purified is collected and dissolved in the ionic liquid is maintained to be lower than the evaporation temperature of the organic material.

The valve 33a and the valve 33b are opened and the supply pump 33 is driven and stored in the supply tank 32 in a state in which the valve 33a and the valve 33b are ready to be charged into the vaporizing part 6 and the collecting part 2, And supplies the liquid organic material to the container 63. Then, the liquid organic material reaches the nozzle 64 by the piping member D3, and is discharged from the discharge port of the nozzle 64 into the container 63. [

The supply amount to the vaporizing portion 6 is controlled by the supply amount control means 3C so that the liquid organic material does not overflow or lack from the accommodation container 63. [ The temperature information detected by the liquid level detection sensor 39a (temperature sensors 391a, 392a, and 393a) is transmitted to the valve controller 39b. The valve controller 39b determines the liquid level of the liquid organic material in the container 63 based on the temperature information received from the liquid level detection sensor 39a. The valve controller 39b lowers the opening degree of the valve 33b to reduce the supply amount or stops the supply pump 33 with closing the valve 33b so as to supply the material Stop. On the contrary, if it is determined that the liquid level has been lowered, the valve controller 39b opens the valve 33b and activates the supply pump 33 to start supplying the liquid organic material if the supply has been stopped. If the supply amount is decreased by adjusting the opening degree of the valve 33b, the valve controller 39b increases the opening degree of the valve 33b to increase the supply amount.

(2-3) Process of circulating the ionic liquid to the collecting section (ionic liquid injection and circulation step)

The discharge valve 74 of the ionic liquid supply tank 71 is closed to fill the tank with the ionic liquid and then the inside of the tank is decompressed by the vacuum pump 73. [ Subsequently, the inside of the housing 21 of the collecting part 2 is decompressed to 10 ^-1 Pa or less by the vacuum pump 23 while the discharge valve 44, the valve 33b and the discharge valve 74 are closed. do. In this state, the discharge valve 74 is opened to supply a predetermined amount of the ionic liquid to the inside of the collecting part 2 at a time, and then the discharge valve 74 is closed.

Then, the outlet valve 44 of the outlet side of the collecting part 2 is opened to circulate the ionic liquid to the collecting part 2 through the pipe member D4, the collecting container 41 and the pipe member D5. Through this cyclical movement, the components inside the collecting part 2 are wetted with the ionic liquid.

(2-4) A step of collecting the vaporized gas of an organic material into an ionic liquid and recrystallizing the same (collecting step (S130), recrystallization step (S140))

When the vaporizer body of the organic material evaporated in the vaporizing section 6 is introduced into the collecting section 2 while the ionic liquid flows while being heated in the collecting section 2, It is collected in the liquid and dissolved. On the other hand, the organic material to be purified is first supersaturated in the collected and dissolved vaporized gas to produce a recrystallized organic material. The organic material recrystallized in the collecting part 2 is appropriately separated from the inside of the collecting container 41 in the process of circulating together with the mixed liquid, and only the mixed material is returned to the collecting part 2.

6 to 9, in the collecting step S130, the ionic liquid flows along the surface of the plurality of blades 25A, 25B, 25C, or 25D disposed across the path in which the vaporizer body is scattered. can do. More specifically, the ionic liquid flows downward along the surface of a plurality of blades 25A, 25B, or 25C that are equally disposed around the vertical axis as shown in Figs. 6 to 8, It is possible to flow by a plurality of blades 25D arranged at the same angle and to rotate or to drop across a path in which the vaporizer body is scattered through the plurality of injection pipes 25E as shown in FIG.

In the recrystallization step (S140), as shown in FIGS. 6 to 9, the vaporized liquid is dissolved in the ionic liquid, and the resulting mixed liquid is circulated along the surfaces of the plurality of blades 25A, 25B, 25C or 25D , And a circulation step of circulating the mixed liquid across the path in which the vaporizer is scattered through the plurality of injection pipes 25E as shown in FIG. On the other hand, in the circulation step, the recrystallized organic material may be separated and recovered in the recovery container 41 (see FIG. 2), and the mixture liquid may be circulated.

The above-described circulation process is repeated periodically or continuously until the impurities in the mixed liquid in the collecting section 2 are supersaturated. The circulation period depends on the amount of ionic liquid initially introduced. It is possible to replace all of the mixed liquid in the collecting part 2 and the circulating part 4 or to replace the periodically circulating mixed liquid with fresh ionic liquid before the impurities are recrystallized in the collecting part 2 You can adjust the number of cycles in the system.

Then, as shown in Fig. 11, in the collecting step S130, the ionic liquid may be applied to the surface of one or more rotary rolls 25F disposed across the path in which the vaporizer body is scattered and flow. On the other hand, the mixture liquid in which the vaporizer body is dissolved in the ionic liquid to be applied to the surface of the rotary roll 25F is peeled from the surface of the rotary roll 25F using the doctor blade 27F located on one side of the rotary roll 25F The recovery step may be further performed.

The recovered mixed liquid is separated into an organic material and an ionic liquid through an appropriate separation process in a reprocessing facility. The ionic liquid is then reused in the purification process. The organic material is refined through an existing inexpensive crude refining process, Can be recycled as a solid organic material.

(2-5) Replacing the recovery container (replacement step)

After the circulation step is repeated a predetermined number of times, the isolated organic material to be isolated is collected separately in the recovery container 41 or all the valves 41a, 41b, 41c attached to the recovery container 41 are closed, (4) and replace with a new recovery container (41).

On the other hand, the purified solid organic material isolated in the recovery vessel 41 is collected, and the remaining mixed liquid is separated into an ionic liquid and an organic material by a distillation method or the like, And the remaining solid organic material is subjected to reprocessing to increase its purity and then used as an organic material.

The internal pressures of the fusion tank 31, the supply tank 32, the vaporizing section 6 and the collecting section 2 of the melting section 3 in the case of continuously purifying the organic material for OLED by the refining apparatus 1, Basically, the relationship is adjusted as follows.

(The fusion tank 31)> (the supply tank 32)> (the vaporizing section 6)> (the collecting section 2)

The supply from the fusion tank 31 to the supply tank 32, the supply from the supply tank 32 to the vaporization unit 6 and the collection of the capture unit 2 are performed without using the supply pump 33 and the transfer pump 42, Is recovered to the recovery container 41 by using the self weight of the liquid organic OLED material, the respective internal pressures are adjusted in this order. It is to be noted that the adjustment of the internal pressure is not performed and the difference in height between the melting tank 31, the supply tank 32, the vaporizing section 6, the collecting section 2 and the recovery container 41, May be adjusted so that the supply using the potential energy may be performed.

In the case of using the feed pump 33 and the feed pump 42 as in this embodiment, the internal pressure is adjusted to the following relationship.

(The piping member D3 on the discharge side of the supply pump 33)> (the collecting section 2, the piping member D4 on the discharge side of the transfer pump 42) (the recovery vessel 41)

When the supply pump 33 and the transfer pump 42 are used, the pump discharge pressure may be higher than the pressure of the tank or the inlet of the vessel, and the fusion tank 31, the supply tank 32 And the pressure in the recovery container 41 are not particularly limited.

The recrystallization mechanism of the organic material according to the present invention will be described below. Since the refining process of the present invention uses a process of recrystallizing the vaporizer body of the organic material for OLED to a solid state by the concentration gradient of the organic material for OLED in the ionic liquid rather than the temperature gradient, The target organic material and the impurities can be separated from each other. At this time, the ionic liquid can be kept heated to a constant temperature in a vacuum atmosphere. That is, the ionic liquid has a very low vapor pressure and can maintain a liquid state without being volatilized even under heating at a certain temperature under vacuum, and this is used as a solvent for organic material purification.

When the vaporized gas of an organic material for an OLED containing an impurity is collected and dissolved in an ionic liquid heated to a predetermined temperature, the organic material forming the mainstream in the ionic liquid firstly reaches the supersaturation. At this time, First, it is recrystallized, and the impurities remain in the dissolved state in the ionic liquid. Considering the reaction in a finer region, the interfacial reaction between the solid and the liquid occurs constantly on the solid surface of the target organic material recrystallized in the ionic liquid. In this case, the solid organic material maintains a homogeneous composition in the solid phase, In order to lower the Gibbs energy, the reaction of discharging impurities to the outside of the solid organic material (ionic liquid) is spontaneously repeated. Through such a mechanism, the solid organic material recrystallized is kept in a pure single phase, and as a result, a high purity organic material can be obtained through a single purification process.

According to the method and apparatus for purifying a gas-phase organic material using the ionic liquid according to the present invention, the following effects are exhibited.

In the refining apparatus 1 of this embodiment, the melting section 3 continuously supplies the solid organic OLED material into the hollow body 61 of the vaporizing section 6 after liquidating it in advance. As a result, it is not necessary to arrange a device for heating and cooling the device for each predetermined amount of tablets as in the case of a conventional tableting device, and continuous purification is possible. Therefore, it is possible to efficiently purify the organic material for OLED even if the amount of purification is increased.

Further, in the refining apparatus 1 of this embodiment, the valve controller 39b determines the remaining amount of the liquid organic material in the hollow body 61 based on the temperature information detected by the liquid level detecting sensor 39a. Then, the valve controller 39b controls the supply pump 33 and the valve 33b based on the determination result. Therefore, even when the tablets are continuously refined, an appropriate amount of the liquid organic material in the body 61 is supplied. Therefore, continuous purification of the organic material for OLED can be performed more stably.

In the refining apparatus 1 of this embodiment, the storage amount controller 38b controls the amount of liquid organic OLED in the supply tank 32 based on the temperature information detected by the liquid level detection sensor 38a of the storage amount control means 38 Determine the amount of material stored. That is, when the amount of storage in the supply tank 32 has decreased, the solid organic OLED material in the melting tank 31 can be melted and supplied to the supply tank 32 based on the determination result. That is, the liquid organic material in the supply tank 32 can be maintained at a predetermined amount or more. Therefore, continuous purification of the organic material for OLED can be performed more stably.

In the refining apparatus 1 of this embodiment, each of the collection containers 41 is detachably connected to the circulation unit 4. Therefore, when the organic material for OLED is continuously refined and the ionic liquid which functions as a refining solvent needs to be replaced, the recovery container 41 can be simply replaced from the circulation unit 4 in a short time, It is not necessary to stop the tablet for a long time. Since the recovery container 41 is detachably connected, when the purified organic OLED material is filled in the recovery container 41, it is possible to stop the circulation once and replace it with another recovery container 41 have. Therefore, in the recovery of the organic material for OLED after purification, it is not necessary to stop the purification, so that the continuous purification of the organic material for OLED can be performed more stably.

Further, in the purification apparatus (1) of this embodiment, since the organic vaporizer body is dissolved in the solvent of the ionic liquid and the target organic material is first supersaturated due to the difference in solubility between the target organic material and the impurities, Organic material can be secured. Also, once the organic material is supersaturated, even if the organic vaporizer is continuously supplied, only the target organic material is recrystallized and recovered, and thus the yield of purification is very high.

Further, in the purification apparatus (1) of this embodiment, since the gaseous organic material is purified by using an ionic liquid as a solvent, the gaseous organic material is melted at a temperature difference or the gas phase organic material is reversely refined by temperature difference There is an advantage that there is little loss during purification.

≪ Modification of Embodiment &

The present invention is not limited to the above-described embodiments, and includes modifications and the like which are described below within the scope of achieving the object of the present invention.

Although one vaporizing section 6 is illustrated as communicating with the collecting section 2 in the above embodiment, a plurality of vaporizing sections 6 are connected around the collecting section 2, and the amount of the organic material purified per circulation cycle Can be increased. In this case, the amount of the ionic liquid circulated in the collecting part 2 must also be correspondingly input.

In the above-described embodiment, the gas-phase organic material is continuously supplied and a certain amount of the ionic liquid is introduced into the circulating medium of the collecting part. However, the number of circulating cycles can be adjusted by replacing the mixed liquid with a new ionic liquid in the middle.

1, the vaporizing portion 6 and the collecting portion 2 are communicated with each other in order to promote the movement of the organic vaporizing body V1 from the vaporizing portion 6 to the collecting portion 2, A structure in which an inert gas V2 is introduced into a path through which the inert gas V2 is introduced and an inert gas that has passed through the trapping section 2 is discharged through a vacuum pump or the like may be selectively added.

In the above embodiment, an example of using the plurality of temperature sensors 381a, 382a, and 383a as the liquid level detecting sensor 38a has been described as an apparatus for detecting the liquid level of the supply tank 32. However, . For example, the liquid level detection sensor 38a may be configured to visually check the liquid level using a level gauge. As a device for detecting the liquid level, a level detector such as a float type, an ultrasonic type, a capacitive type, a pressure type or an optical type can be applied.

In the above embodiment, an example in which the plurality of temperature sensors 391a, 392a, and 393a of the liquid level detecting sensor 39a are used as the apparatus for detecting the liquid level of the vaporizing section 6 has been described. However, . For example, the liquid level detection sensor 39a may be configured to visually check the liquid level using a level gauge. As a device for detecting the liquid level, a level detector such as a float type, an ultrasonic type, a capacitance type, a pressure type or an optical type may be applied.

In the above embodiment, the feedback control based on the liquid level detection is described as a method of controlling the supply amount of the liquid organic OLED material to the vaporizing part 6, but the present invention is not limited to this embodiment. For example, a configuration may be employed in which a flow meter is provided on the discharge side of the valve 33b, and the supply amount of the liquid organic OLED material to the vaporizing part 6 is controlled based on the measured value in the flow meter. In addition, the relationship between the pump stroke of the supply pump 33 and the flow rate at the time of flowing the organic material for OLED may be grasped in advance and the supply amount may be controlled by adjusting the pump stroke. Alternatively, . The liquid level detection by the liquid level detection sensor 39a is combined with the control by the flow meter and the control of the pump stroke of the feed pump 33 so that the feed pump 33 and the valve (33b) may be controlled.

The internal structure of the trapping portion of the present invention is not particularly limited. In the above embodiment, the ionic liquid is flowed by the self-weight as a flow means of the ionic liquid, but various modifications are possible in a manner maximizing the contact between the vaporized gas of the organic material and the ionic liquid.

In the above embodiments, quartz glass is mainly used as an inactive material for the OLED organic material. However, the present invention is not limited thereto. For example, stainless steel, tantalum, tungsten, molybdenum, titanium, zirconia, carbon, alumina, boron nitride, silicon nitride, and Teflon.

Further, the material of the vaporizing part and the collecting part is not limited to a material which is inactive to the organic material for the OLED as a whole. It may be made of a material which is inactive only for the portion where the organic material for OLED contacts and other materials for the other portions.

On the other hand, the heating means and the heating method for heating the vaporizing portion, the collecting portion and the circulating portion are not limited to those described in the above embodiment. Examples of the heating method include a resistance heating method (metal system, nonmetal system, etc.), a light heating method (infrared heating method, arc radiation heating, laser radiation heating and the like), an induction heating method, a plasma heating method, . For example, in the case of heating by the induction heating method, the material of the vaporizing portion and the collecting portion may be made of a material that generates heat by electromagnetic induction such as stainless steel.

In the above embodiment, the recovery pump is used as the recovery pump. However, the present invention is not limited to this. For example, the recovery container 41 of the circulation part may be disposed at a lower position than the mixing part so as to flow into the recovery container by using the weight of the liquid organic OLED material itself, without interposing a recovery pump.

In addition to the low molecular weight organic light emitting materials for manufacturing OLED devices, the organic materials applied to the above embodiments include organic TFT materials, organic solar cell materials, and organic semiconductor materials. Therefore, the present invention can be used for purification of organic materials applied to various fields as described above.

1: Purification device 2: Collecting part
3: fusion unit 4: circulation unit
5: vaporization part 7: ionic liquid supply part
8: Temperature controller

Claims (16)

A melting portion for melting a solid organic material containing an impurity,
A vaporizing portion for vaporizing the liquid organic material produced in the melting portion,
And a collecting part for collecting the vaporized gas by bringing the vaporized gas generated by the vaporized part into contact with the flowing ionic liquid,
Characterized in that the trapping portion first superposes the organic material to be purified in the vaporized gas collected and dissolved in the ionic liquid to generate a recrystallized solid organic material. . The method according to claim 1,
The collecting unit collects,
A housing connected to the vaporizing portion so as to communicate with the vaporizing portion,
A plurality of blades disposed in the housing across a path through which the vaporizer body spans,
Ionic liquid supply means for supplying the ionic liquid to flow along the surface of the blades, and
And a storage means for storing the mixed liquid obtained by dissolving the vaporizer in the ionic liquid and the recrystallized organic material. The method of claim 2,
Further comprising a circulation unit for circulating the mixed liquid from the storage unit along the surface of the plurality of blades. The method according to claim 1,
The collecting unit collects,
A housing communicating with the vaporizing portion,
Ionic liquid supply means for supplying the ionic liquid so that the vaporizer body falls across a path through which the vaporizer body sprays, and
And a storage means for storing the mixed liquid obtained by dissolving the vaporizer in the ionic liquid and the recrystallized organic material. The method of claim 4,
Further comprising a circulation unit for circulating the mixed liquid from the storage unit and dropping the vaporized liquid across the path through which the vaporizer is scattered. The method according to claim 3 or 5,
Wherein the circulation unit discharges the mixed liquid in the storage unit and the recycled solid organic material to the outside of the storage unit and then separates and recovers the recrystallized solid organic material and collects the mixed liquid, Wherein the ionic liquid is used to purify the gas-phase organic material. The method according to claim 1,
The collecting unit collects,
A housing connected to the vaporizing portion so as to communicate with the vaporizing portion,
One or more rotating rolls disposed in the housing across a path through which the vaporizer body spans, and
And an ionic liquid storage portion disposed below the rotary roll and supplying the ionic liquid to the surface of the rotary roll. The method of claim 7,
And a doctor blade for dissolving the mixed liquid generated by dissolving the vaporizer in the ionic liquid from the surface of the rotary roll is provided on one side of the rotary roll. . A melting step of melting a solid organic material containing impurities,
A vaporization step of vaporizing the liquid organic material produced in the melting step,
A collecting step of collecting the vaporized gas by bringing the vaporized gas of the organic material into contact with the flowing ionic liquid, and
And a recrystallization step of initially recrystallizing the organic material to be purified in the vaporized gas collected and dissolved in the ionic liquid to produce a recrystallized solid organic material. The method of claim 9,
Wherein in said collecting step said ionic liquid flows along a surface of a plurality of blades disposed across a path through which said vaporizer body spans. The method of claim 10,
Wherein the recrystallization step further comprises a circulation step of circulating the mixed liquid generated by dissolving the vaporizer in the ionic liquid along the surface of the plurality of blades. . The method of claim 9,
Wherein in the collecting step, the ionic liquid flows down across the path of scattering of the vaporizer body. The method of claim 12,
Further comprising a circulation step of circulating the mixed liquid generated by dissolving the vaporizer in the ionic liquid across the path in which the vaporizer is scattered in the recrystallization step. Way. The method according to claim 10 or 13,
Wherein the circulating step comprises filtering the recrystallized solid organic material and circulating the mixed liquid. The method of claim 9,
Wherein in the collecting step, the ionic liquid flows on the surface of one or more rotary rolls disposed across a path through which the vaporizer is scattered, and flows. 16. The method of claim 15,
Further comprising the step of peeling off the mixed liquid generated by dissolving the vaporizer in the ionic liquid using a doctor blade from the surface of the rotating roll.

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