WO2013065626A1 - Appareil de purification d'une matière organique et procédé de purification d'une matière organique - Google Patents

Appareil de purification d'une matière organique et procédé de purification d'une matière organique Download PDF

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Publication number
WO2013065626A1
WO2013065626A1 PCT/JP2012/077852 JP2012077852W WO2013065626A1 WO 2013065626 A1 WO2013065626 A1 WO 2013065626A1 JP 2012077852 W JP2012077852 W JP 2012077852W WO 2013065626 A1 WO2013065626 A1 WO 2013065626A1
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Prior art keywords
organic material
organic
cylinder
element material
collector
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PCT/JP2012/077852
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English (en)
Japanese (ja)
Inventor
芳賀　亮
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出光興産株式会社
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Application filed by 出光興産株式会社 filed Critical 出光興産株式会社
Priority to KR1020147012663A priority Critical patent/KR20140084165A/ko
Publication of WO2013065626A1 publication Critical patent/WO2013065626A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/0011—Heating features
    • B01D1/0017—Use of electrical or wave energy
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/0088—Cascade evaporators
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B63/00—Purification; Separation; Stabilisation; Use of additives
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
    • H10K71/00—Manufacture or treatment specially adapted for the organic devices covered by this subclass
    • H10K71/311—Purifying organic semiconductor materials

Definitions

  • the present invention relates to an organic material purification apparatus and an organic material purification method.
  • organic material used as an electronic material or an optical material is purified to a high purity because its purity may greatly affect the performance.
  • an organic material a material used for an organic electroluminescence element (hereinafter referred to as an organic EL element) that has been actively researched and developed in recent years can be given. If impurities are mixed in materials used for organic EL elements (hereinafter referred to as organic EL element materials), the impurities may trap carriers (electrons and holes) or cause quenching. In other words, the light emission intensity, light emission efficiency, and durability of the organic EL element are reduced.
  • the purification apparatus described in Patent Document 1 includes a cylindrical evaporator (evaporator) that evaporates and evaporates the organic EL element material, and a cylindrical collector (collector) that condenses and collects evaporated gas.
  • the temperature of the collection part is comprised so that it may fall substantially stepwise or continuously toward the downstream.
  • a predetermined amount of a material for an organic EL element (N, N′-di- (naphthalen-1-yl) -N, N′-diphenyl-benzidine, NPB) is used.
  • NPB N′-di- (naphthalen-1-yl) -N, N′-diphenyl-benzidine
  • the placed glass boat is placed in the evaporation section, the evaporation section and the collection section are each heated to a predetermined temperature, the inside of the apparatus is depressurized under a predetermined pressure, and purification is performed. After purification, the temperature of the collection part is lowered and NPB is recovered as a solid.
  • purification apparatus described in patent document 2 is an apparatus which heats and sublimates the material for organic EL elements by an electromagnetic induction system, sublimates the material with which the cylindrical sublimation part was charged, and is cylindrical. Condensation or coagulation is collected at the collection part. After the refining operation, the target material is recovered by removing the collection part.
  • purification apparatus described in patent document 3 the solid mixture charged to the sublimation tank is sublimated under reduced pressure, vapor
  • Patent Document 1 to Patent Document 3 a predetermined amount of the organic EL element material is accommodated in the apparatus for each purification, and purification is performed under conditions of a predetermined temperature and a predetermined pressure. Thereafter, the organic EL element material is collected. That is, it is necessary to perform purification by batch processing. Therefore, in the refining apparatuses of Patent Documents 1 to 3, the amount of organic EL element material that can be processed by one purification is limited, and if the processing amount of the organic EL element material is increased, the organic EL element material may be evaporated. , Have a tremendous amount of time to sublimate and cool. This is for avoiding rapid temperature rise and cooling and preventing decomposition of the organic EL element material.
  • An object of the present invention is to provide an organic material purification apparatus and an organic material purification method capable of efficiently purifying an organic material even if the amount of purification is increased.
  • the organic material refining device of the present invention comprises: A first cylinder that is supplied with an organic material therein, and an evaporator that is disposed outside the first cylinder and includes a heater that evaporates the supplied organic material; A second cylinder that communicates with the first cylinder of the evaporator, and a temperature adjustment heater that is disposed outside the second cylinder and adjusts the temperature of the second cylinder, evaporates in the evaporator A collector for liquefying and collecting the gaseous organic material on the inner surface of the second cylinder, And a liquefied continuous supply device for liquefying a solid organic material and continuously supplying the liquid organic material into the evaporator.
  • the liquefied continuous supply device continuously supplies the solid organic material into a liquid state and then continuously supplies it to the evaporator in the device main body.
  • continuous supplying not only means that the organic material is continuously supplied, but also the organic material is supplied in a predetermined cycle or a different cycle in a state in which the refining apparatus is continuously operated without being stopped. This also means that supply and stop are performed continuously.
  • the organic material refining apparatus of the present invention since the liquid organic material can be continuously supplied to the evaporator, it is necessary to heat and cool the apparatus for every predetermined amount of refining as in the conventional refining apparatus. And purification can be performed continuously. Therefore, according to the present invention, the organic material can be efficiently purified even if the amount of purification is increased.
  • the evaporator includes a receiving portion that receives the liquid organic material supplied from the liquefaction continuous supply device to the inside of the first cylinder,
  • the liquefaction continuous supply unit detects the liquid level of the liquid organic material in the container, and controls the supply amount of the liquid organic material based on the detected liquid level detection signal. It is preferable that a means is provided.
  • the supply amount control means detects the liquid level of the organic material in the container and controls the supply amount from the continuous liquefaction feeder to the evaporator. Therefore, even if it refine
  • the second cylinder of the collector is configured by connecting a plurality of collector cylinders, It is preferable that a dam plate is formed at a connecting portion between the plurality of collecting cylinders.
  • the second cylinder is configured by connecting a plurality of collection cylinders, by adjusting the temperature of each collection cylinder to be different, an organic material with high purity and Accurately classify and collect organic materials with low purity.
  • the collection cylinder can be separated after purification and can be easily cleaned.
  • the dam plate is formed in the connection part of collection cylinders, it can prevent mixing the organic material after the refinement
  • a discharge hole for discharging the collected liquid organic material is formed in the second cylinder of the collector, It is preferable that a collection container is detachably connected to the discharge hole.
  • the recovery container is connected to the discharge hole formed in the second cylinder. Therefore, even if the organic material is continuously purified and the purified material collected by the second cylinder increases, it can be collected in a collection container outside the collector. Further, since the recovery container is detachably connected, when the inside of the recovery container is filled with the purified organic material, it is possible to stop the recovery once and switch to another recovery container for connection. Therefore, according to the present invention, there is no need to stop the purification when recovering the organic material after purification, so that continuous purification of the organic material can be performed more stably.
  • an inclined surface that is inclined downward toward the discharge hole is formed on the inner surface of the second cylindrical body of the collector.
  • the liquid organic EL element material after collection is transmitted through the inner surface and the inclined surface of the second cylinder, It is efficiently collected in the discharge hole.
  • the collected liquid organic material is recovered in the recovery container as described above. Therefore, according to the present invention, the organic material after purification can be efficiently recovered.
  • the collector is inclined so as to rise or descend from the evaporator side toward the collector side
  • the discharge hole is formed on the evaporator side of the second cylindrical body when the collector is inclined so as to be inclined upward, and the collector is inclined so as to be inclined downward Preferably, it is formed on the collector side.
  • the collector is inclined and the discharge hole is formed on the evaporator side or the collector side. Therefore, the liquid organic EL element material after collection is Can be efficiently collected in the discharge hole at a low position. In addition, by tilting in this way, the liquid organic EL element material after collection can be efficiently collected in the discharge hole even if the tilted surface is not formed on the inner surface of the second cylinder. Therefore, the manufacturing cost of the second cylinder can be reduced.
  • the method for purifying the organic material of the present invention comprises: A liquefaction step of heating and liquefying the solid organic material under reduced pressure; A supply step of continuously supplying the liquid organic material liquefied in the liquefaction step into the first cylinder; An evaporation step of evaporating the liquid organic material supplied to the inside of the first cylinder in the supply step with a heater disposed outside the first cylinder; The gaseous organic material evaporated in the evaporation step is condensed and collected on the inner surface of the second cylinder that is communicated with the first cylinder and is temperature-adjusted by a temperature adjusting heater disposed outside. And a collecting step.
  • the solid organic material is liquefied in the liquefaction step, the liquid organic material liquefied in the supply step is supplied to the inside of the first cylinder, and the evaporation step and the collection step are performed. carry out.
  • a liquid organic material can be continuously supplied to the 1st cylinder which implements an evaporation process. Therefore, it is not necessary to heat and cool the apparatus for every predetermined amount of purification as in the conventional purification method, and the purification can be performed continuously. Therefore, according to the present invention, the organic material can be efficiently purified even if the amount of purification is increased.
  • the organic material refining method of the present invention the organic material is continuously purified, and even if the purified material collected by the second cylinder increases, it can be recovered in the recovery container. Further, since the recovery container is detachably connected, when the inside of the recovery container is filled with the purified organic material, it is possible to stop the recovery once and switch to another recovery container for connection. Therefore, according to the present invention, there is no need to stop the purification when recovering the organic material after purification, so that continuous purification of the organic material can be performed more stably.
  • the refining device 1 includes a device main body 2 for purifying an organic material, a liquefied continuous supply device 3 for supplying the organic material to the device main body 2, a recovery device 4 for recovering the purified organic material, and the inside of the device main body 2 under reduced pressure. And a temperature controller 8 for controlling the temperature of the apparatus main body 2.
  • a device main body 2 for purifying an organic material
  • a liquefied continuous supply device 3 for supplying the organic material to the device main body 2
  • a recovery device 4 for recovering the purified organic material
  • a temperature controller 8 for controlling the temperature of the apparatus main body 2.
  • the device main body 2 is formed in a cylindrical shape in which an evaporator 6 and a collector 7 are arranged adjacent to each other in the horizontal direction, and both ends of the cylindrical device main body 2 are closed by lids 21 and 22. ing. Moreover, as shown in FIG. 1, the liquefaction continuous supply device 3 is connected to the end of the apparatus body 2 on the evaporator 6 side, and the vacuum pump 5 is connected to the end of the collector 7 side. Yes.
  • the vacuum pump 5 is provided with a piping member via a valve 5 a, and the piping member is inserted into the apparatus main body 2.
  • the pressure in the apparatus main body 2 is set to 10 ⁇ 1 Pa or less.
  • a trap device (not shown) is interposed between the apparatus main body 2 and the vacuum pump 5.
  • the organic EL element material supplied from the liquefied continuous supply device 3 is evaporated by the evaporator 6, and the evaporated gaseous organic EL element material is captured by suction of the vacuum pump 5. It flows into the collector 7 and is liquefied and collected by the collector 7.
  • the organic EL element material to be purified flows from the evaporator 6 side to the collector 7 side.
  • the side of the apparatus main body 2 where the evaporator 6 is disposed is the upstream side
  • the side of the apparatus main body 2 where the collector 7 is disposed is the downstream side.
  • the material of the apparatus main body 2 is preferably composed of a material that is inactive with respect to the organic EL element material. This is to prevent the organic EL element material from being decomposed or undergoing modification such as polymerization under the conditions during purification (temperature, pressure, etc.).
  • the apparatus main body 2 is made of quartz glass.
  • the evaporator 6 is disposed on the upstream side of the apparatus main body 2.
  • the evaporator 6 includes a first cylindrical body 61, a heater 62 disposed outside the first cylindrical body 61, a housing portion 63 disposed inside the first cylindrical body 61, and the first cylindrical body 61. And a weir plate 68 formed at a connection position with respect to the collector 7.
  • the first cylinder 61 is formed in a cylindrical shape.
  • An accommodating portion 63 that receives a liquid organic EL element material is disposed at a substantially central portion inside the cylinder of the first cylinder 61.
  • the accommodating part 63 is formed in the dish shape provided with the square-plate-shaped bottom face and the side surface which stands up out of the surface from the periphery of this bottom face, for example.
  • a nozzle 64 having a discharge port directed toward the storage portion 63 is disposed above the storage portion 63.
  • the nozzle 64 discharges the liquid organic EL element material supplied from the liquefaction continuous supply device 3 toward the dish-shaped storage portion 63.
  • the heater 62 is configured by a heating wire heater or the like, and is arranged in an annular shape outside the first cylinder 61.
  • the dam plate 68 is an annular member that closes a part of the end opening surface of the first cylinder 61.
  • the dam plate 68 is joined to the end of the first cylinder 61 to prevent the organic EL element material supplied into the first cylinder 61 from flowing directly into the collector 7, The organic EL element material collected by the collector 7 is prevented from flowing into the evaporator 6 side.
  • the material of the first cylinder 61, the accommodating portion 63, and the dam plate 68 is preferably made of a material that is inert with respect to the organic EL element material, and is made of quartz glass in the first embodiment.
  • the collector 7 is disposed on the downstream side of the apparatus main body 2.
  • the collector 7 includes a cylindrical second cylinder 71 and a temperature adjustment heater 72 disposed outside the second cylinder 71.
  • a plurality of dam plates 78 which are annular members similar to the dam plate 68 are formed.
  • the second cylinder 71 is divided into a plurality of collection chambers by these barrier plates 78.
  • the plurality of collection chambers are formed continuously in the horizontal direction toward the downstream side and communicate with each other. In 1st embodiment, it is divided into three collection chambers, ie, the 1st collection chamber 71A, the 2nd collection chamber 71B, and the 3rd collection chamber 71C in order from the upstream.
  • Each collection chamber 71A, 71B, 71C condenses the gaseous organic EL element material evaporated by the evaporator 6 and collects it as a liquid organic EL element material.
  • the temperature adjustment heater 72 is configured by a heating wire heater or the like, and is arranged in an annular shape outside the second cylinder 71. The temperature adjustment heater 72 can independently adjust the temperature inside each collection chamber 71A, 71B, 71C.
  • a quartz tube 73 for discharging the collected liquid organic EL element material to the outside is connected to the collector 7. One end side of the quartz tube 73 is connected to the lower part of each collection chamber 71A, 71B, 71C.
  • the recovery device 4 is connected to the other end side of the quartz tube 73.
  • the quartz tube 73 communicates with each of the collection chambers 71A, 71B, 71C, and the inside of the quartz tube 73 serves as a discharge hole 73a for discharging the collected organic EL element material.
  • An inclined surface 74 is preferably formed on the lower inner surface of each collection chamber 71A, 71B, 71C.
  • the inclined surface 74 has a downward slope from the dam plate 78 side toward the discharge hole 73a.
  • the liquid organic EL element material collected in each of the collection chambers 71A, 71B, 71C flows through the inclined surface 74 and flows into the discharge hole 73a of the quartz tube 73.
  • the weir plate 78 prevents the purified organic EL element material collected in each of the collection chambers 71A, 71B, 71C from flowing into the adjacent collection chamber.
  • the aforementioned dam plate 68 is formed at the boundary between the first collection chamber 71A and the evaporator 6, and the dam plate 68 prevents mixing of the organic EL element material before and after purification.
  • a dam plate 78 is also formed on the downstream side of the third collection chamber 71 ⁇ / b> C to prevent the collected organic EL element material from flowing into the lid portion 22 that closes the downstream end of the apparatus main body 2.
  • the material of the second cylinder 71 and the dam plate 78 is preferably made of a material that is inert to the organic EL element material, and is made of quartz glass in the first embodiment.
  • the temperature controller 8 is measured by a temperature sensor 81 that measures the temperature inside the evaporator 6, a temperature sensor 82 that measures the temperature inside the collector 7, and the temperature sensors 81 and 82. And a control unit 83 that controls the heater 62 and the temperature adjusting heater 72 based on the temperature information.
  • the temperature sensor 81 is disposed inside the first cylinder 61, and the temperature sensor 82 is disposed inside the second cylinder 71 and is connected to a control unit 83 disposed outside the apparatus main body 2.
  • the temperature information measured by the temperature sensors 81 and 82 is sent to the control unit 83.
  • each temperature sensor 82 is arranged corresponding to the position of each of the collection chambers 71A, 71B, 71C.
  • a temperature sensor 82 arranged for each of the collection chambers 71A, 71B, 71C sends temperature information to the control unit 83.
  • a thermocouple is used.
  • the control unit 83 is connected to the heater 62 and the temperature adjustment heater 72, and controls heating by the heater 62 and the temperature adjustment heater 72 based on temperature information input from the temperature sensors 81 and 82.
  • control unit 83 independently controls the temperature adjustment heater 72 for each of the collection chambers 71A, 71B, 71C.
  • the controller 83 controls the temperature adjustment heater 72 so that the temperature varies continuously or stepwise from the first collection chamber 71A side to the third collection chamber 71C side.
  • the shielding section 23 is provided on the upstream side and the downstream side of the apparatus main body 2 and outside the collection chamber for the organic EL element material to be purified. Leakage of the first cylinder 61 and the temperature drop in the second cylinder 71 is prevented.
  • Two upstream shielding portions 23 ⁇ / b> A are provided inside the first cylinder 61 inside the lid portion 21 of the apparatus main body 2 and upstream of the housing portion 63.
  • Two downstream shielding portions 23B are provided inside the second cylindrical body 71 on the inner side of the lid portion 22 of the apparatus main body 2 and on the downstream side of the weir plate 78 of the third collection chamber 71C.
  • the shielding part 23 is configured by connecting a plurality of circular shielding plates 231.
  • three shielding plates 231 are connected, and the connected shielding plates 231 are separated from each other by a predetermined dimension.
  • the diameter of the shielding plate 231 is preferably such that the shielding portion 23 is formed to have substantially the same dimensions as the inner diameters of the first cylindrical body 61 and the second cylindrical body 71, and when the shielding portion 23 is installed, the shielding plate 231.
  • the gap between the side surface and the inner surfaces of the first cylinder body 61 and the second cylinder body 71 can be reduced.
  • FIG. 2 shows a plan view of the shielding part 23.
  • Each shielding plate 231 is formed with a plurality of through holes 232 penetrating the front and back.
  • the three shielding plates 231 are connected so that the through hole 232 of a certain shielding plate 231 does not overlap with the position of the through hole 232 of another shielding plate 231 adjacent thereto.
  • the plurality of through holes 232 are formed radially from substantially the center of the shielding plate 231, and the through holes 232 are overlapped by connecting the shielding plates 231 while shifting the phase in the rotational direction. It is preventing.
  • a through hole 233 and a through hole 234 other than the through hole 232 are formed in each shielding plate 231.
  • the through hole 233 and the through hole 234 are formed so as to overlap each other when the shielding plate 231 is connected so that the through hole 232 does not overlap as described above, and the member can be inserted through the through hole 233 or the through hole 234. Yes.
  • the through hole 233 is used to insert the temperature sensor 81 and the temperature sensor 82 from the outside of the apparatus main body 2 to the inside.
  • the through-hole 234 is used for inserting a pipe member L3 for supplying a liquid organic EL element material from the liquefied continuous supply device 3 to the evaporator 6 from the outside of the apparatus main body 2 to the inside.
  • the material of the shielding part 23 is comprised with a material inactive with respect to the material for organic EL elements, and is comprised with stainless steel in 1st embodiment.
  • the continuous liquefaction feeder 3 liquefies the solid organic EL element material, and places the liquid organic EL element material in the housing 63 installed in the evaporator 6. Supply continuously.
  • the continuous liquefaction feeder 3 stores a raw material replenisher 3 ⁇ / b> A that liquefies solid organic EL element material, a liquid organic EL element material provided on the discharge side of the liquefaction tank 31, and supplies it to the evaporator 6.
  • a supply unit 3B and a supply amount control means 3C provided on the discharge side of the supply tank 32 and controlling the supply amount to the evaporator 6 are provided.
  • continuous supplying not only means that the organic material is continuously supplied, but also the organic material is supplied in a predetermined cycle or in a state where the refining apparatus is continuously operated without being stopped. It also means that supply and stop are continuously performed at different periods, and in this embodiment, supply and stop of the organic EL element material are controlled by the supply amount control means 3C.
  • the raw material replenisher 3A includes a hopper 34 for supplying a solid organic EL element material, and the supplied solid organic EL element.
  • a liquefaction tank 31 for storing the material for use and the liquefied liquid organic EL element material, a vacuum pump 36a for reducing the pressure inside the liquefaction tank 31, and an infrared heater 35 for heating the liquefaction tank 31.
  • the liquefaction tank 31 is composed of a pressure vessel, and the solid organic EL element material is liquefied inside the liquefaction tank 31.
  • the material of the liquefaction tank 31 is preferably made of a material that is inert with respect to the organic EL element material.
  • the liquefaction tank 31 is made of quartz glass.
  • the hopper 34 is connected to the liquefaction tank 31 by a piping member L1, and a valve 31a is provided in the middle of the piping member L1.
  • the supply of the solid organic EL element material from the hopper 34 into the liquefaction tank 31 is controlled by opening and closing the valve 31a.
  • the material of the hopper 34 is preferably made of a material that is inert with respect to the organic EL element material.
  • the material of the hopper 34 is made of quartz glass.
  • the lid 34a is attached to the upper portion of the hopper 34 so as to be opened and closed, and the solid organic EL element material is prevented from being photodegraded and oxidized by being in contact with air.
  • the vacuum pump 36a is connected to the liquefaction tank 31 by a piping member, and a valve 31c is provided in the middle of the piping member.
  • the pressure in the liquefaction tank 31 is set to 10 ⁇ 1 Pa or less.
  • the infrared heater 35 is disposed so as to surround the outer periphery of the liquefaction tank 31.
  • the infrared heater 35 is connected to the temperature controller 8 described above.
  • the infrared heater 35 heats the liquefaction tank 31 so that the solid organic EL element material supplied into the liquefaction tank 31 reaches a temperature at which it liquefies. Specifically, the inside of the liquefaction tank 31 is heated to the melting point of the organic EL element material to be liquefied.
  • the temperature of the liquefaction 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 heating by the infrared heater 35 based on the received temperature information.
  • the supply unit 3B is, as shown in FIG. 3, a supply tank 32 that temporarily stores liquid organic EL element material until it is supplied to the evaporator 6, A vacuum pump 36b for depressurizing the inside of the supply tank 32, an infrared heater 37 for heating the supply tank 32, and a storage amount control for detecting and controlling the amount of liquid organic EL element material stored in the supply tank 32 Means 38.
  • the supply tank 32 is disposed on the discharge side of the liquefaction tank 31.
  • the supply tank 32 is composed of a pressure vessel.
  • the material of the supply tank 32 is preferably made of a material that is inert with respect to the organic EL element material.
  • the supply tank 32 is made of quartz glass.
  • the discharge side of the liquefaction tank 31 and the reception side of the supply tank 32 are connected by a piping member L2.
  • a valve 31b is provided in the middle of the piping member L2. The valve 31 b controls the replenishment of the liquid organic EL element material from the liquefaction tank 31 to the supply tank 32.
  • the supply tank 32 is installed at a position lower than the liquefaction tank 31.
  • a piping member L3 is connected to the discharge side of the supply tank 32. As shown in FIGS. 1 and 4, the piping member L ⁇ b> 3 is inserted to the inside of the evaporator 6, and the tip thereof is connected to the nozzle 64 above the housing portion 63. A heater (not shown) is disposed on the outer periphery of the piping members L2, L3. Therefore, solidification of the organic EL element material in the piping members L2 and L3 can be prevented.
  • the vacuum pump 36b is connected to the supply tank 32 by a piping member, and a valve 32a is provided in the middle of the piping member.
  • the pressure in the supply tank 32 is set to 10 ⁇ 1 Pa or less.
  • the supply tank 32 may be filled with nitrogen after being evacuated by the vacuum pump 36b.
  • the infrared heater 37 is disposed so as to surround the outer periphery of the supply tank 32.
  • the infrared heater 37 is connected to the temperature controller 8 described above.
  • the infrared heater 37 heats the supply tank 32 so that the temperature of the organic EL element material accommodated in the supply tank 32 does not solidify. Specifically, the inside of the supply tank 32 is heated to the melting point of the organic EL element material to be liquefied.
  • the organic EL element material supplied from the liquefaction tank 31 without being liquefied can also be liquefied 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 heating by the infrared heater 37 based on the received temperature information.
  • the storage amount control means 38 is a liquid level detection sensor 38a for detecting the liquid level of the liquid organic EL element material in the supply tank 32, and the storage amount based on the information detected by the liquid level detection sensor 38a. And a storage amount controller 38b for controlling. Information detected by the liquid level detection sensor 38a is transmitted to the storage amount controller 38b.
  • the liquid level detection sensor 38a includes three temperature sensors 381a, 382a, and 383a. As shown in FIG. 3, a temperature sensor 381a is disposed at the lower portion with respect to the height direction of the supply tank 32, a temperature sensor 382a is disposed at the middle portion, and a temperature sensor 383a is disposed at the upper portion.
  • the storage amount controller 38b receives the temperature information detected by the liquid level detection sensor 38a, and determines the storage amount of the liquid organic EL element material inside the supply tank 32 based on this temperature information.
  • the detected temperature differs between the temperature sensor 383a positioned above the liquid level and the temperature sensors 381a and 382a positioned below the liquid level. .
  • the storage amount controller 38b determines the liquid level and the storage amount based on the difference in the detected temperature.
  • the storage amount controller 38b displays the determination result of the storage amount on the display means 38c constituted by a display or the like.
  • the storage amount controller 38b determines that the liquid organic EL element material necessary for continuous purification is not stored in the supply tank 32, the storage means 38b displays the fact on the display means 38c. Further, an alarm sound may be emitted. The operator can determine whether or not the organic EL element material should be liquefied in the liquefaction tank 31 and additionally supplied to the supply tank 32 based on the display and alarm sound.
  • the storage amount controller 38b may be connected to the temperature controller 8, the vacuum pumps 36a and 36b, and the valves 31a, 31b, 31c, and 32a, and the storage amount control means 38 may include these. These operations may be controlled by the storage amount controller 38b, and additional supply to the supply tank 32 may be automatically performed.
  • the supply amount control unit 3C is disposed on the discharge side of the supply tank 32, and controls the amount of liquid organic EL element material supplied to the evaporator 6.
  • FIG. 4 shows the supply amount control means 3C.
  • the supply amount control means 3C includes a supply pump 33 provided in the middle of the piping member L3 connected to the discharge side of the supply tank 32, a valve 33a provided between the supply tank 32 and the supply pump 33, and a supply pump 33. And a valve 33 b provided between the evaporator 6, a liquid level detection sensor 39 a disposed in the accommodating portion 63 in the evaporator 6, and a valve controller 39 b connected to the liquid level detection sensor 39 a.
  • the supply pump 33, the valve 33a and the valve 33b control the supply amount of the liquid organic EL element material discharged from the supply tank 32 and supplied to the evaporator 6.
  • the supply amount control means 3C may not include the supply pump 33.
  • the liquid level detection sensor 39a detects the remaining amount of the liquid organic EL element material remaining in the storage unit 63.
  • the liquid level organic EL element in the storage unit 63 is used.
  • the liquid level of the material used is detected.
  • 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, similar to the liquid level detection sensor 38a described above. As shown in FIG. 4, a temperature sensor 391a is arranged at the lower part with respect to the depth direction of the housing part 63, a temperature sensor 392a is arranged at the middle part, and a temperature sensor 393a is arranged at the upper part.
  • the valve controller 39b receives the temperature information detected by the liquid level detection sensor 39a, and determines the liquid level and the remaining amount of the liquid organic EL element material inside the storage unit 63 based on the temperature information.
  • the detected temperature differs between the temperature sensor 393a positioned above the liquid level and the temperature sensors 391a and 392a positioned below the liquid level.
  • the valve controller 39b determines the remaining amount based on the detected temperature difference.
  • the valve controller 39b is connected to a display means 39c constituted by a display or the like, and can display the determination result 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, and controls the supply pump 33 and the valve 33b so that the remaining amount of the liquid organic EL element material in the housing portion 63 is within a predetermined range. To do. In this way, the valve controller 39b automatically controls the supply of the liquid organic EL element material to the evaporator 6.
  • the recovery device 4 includes three recovery devices 4A, a recovery device 4B, and a recovery device 4C that are connected to the three discharge holes 73a.
  • the collection device 4A is connected to the discharge hole 73a of the first collection chamber 71A
  • the collection device 4B is connected to the discharge hole 73a of the second collection chamber 71B
  • the collection device 4C is connected to the third collection chamber 71B. It is connected to the discharge hole 73a of the collection chamber 71C. Since the recovery devices 4A, 4B, and 4C have almost the same configuration, the recovery device 4A will be described below, and the description of the other recovery devices 4B and 4C will be omitted. As shown in FIG.
  • the recovery device 4A includes a discharge valve 44 that controls the discharge amount of the purified liquid organic EL element material discharged from the first collection chamber 71A, and the discharged liquid state A transfer pump 42 for transferring the organic EL element material, a recovery container 41 for recovering and storing the liquid organic EL element material, and a vacuum pump 43 for reducing the pressure inside the recovery container 41. .
  • the discharge valve 44 is connected to the other end side of the quartz tube 73 connected to the first collection chamber 71A.
  • the discharge valve 44 and the collection container 41 are connected by a piping member L4.
  • a transfer pump 42, a valve 42a, and a valve 41a are provided in this order from the discharge valve 44 side.
  • the collection container 41 and the vacuum pump 43 are connected by a piping member, and a valve 41b is provided in the middle of the piping member.
  • the pressure in the collection container 41 is set to 10 ⁇ 1 Pa or less.
  • the organic EL element material may be recovered in a state where the recovery container 41 is filled with nitrogen.
  • the recovered liquid organic EL element material is cooled in the recovery container 41.
  • the collection container 41 is detachably formed between the valve 41 a and the valve 42 a and between the valve 41 b and the vacuum pump 43. Therefore, the recovery container 41 can be separated from the recovery device 4A in a state where the recovery container 41 is sealed. After separation, an empty collection container 41 prepared separately can be attached.
  • the collection container 41 is preferably made of a material that is inert to the organic EL element material in order to store the organic EL element material therein.
  • the transfer pump 42 is connected between the discharge valve 44 and the valve 42 a, and transfers the liquid organic EL element material discharged from the discharge hole 73 a to the collection container 41.
  • a branch point J1 is formed in the middle of the piping member L4 connecting the transfer pump 42 and the valve 42a.
  • a junction J2 is formed in the middle of the piping member L4 connecting the transfer pump 42 and the discharge valve 44.
  • the branch point J1 and the junction point J2 are connected by the piping member L5 via the valve 42b.
  • a so-called minimum flow line is formed around the transfer pump 42 by adopting such a pipe configuration.
  • the valve 42a is closed and the valve 42b is opened, so that the liquid organic EL element material discharged from the transfer pump 42 is passed from the branch point J1 through the valve 42b.
  • the line is formed so as to return to the junction point J2 and to flow into the transfer pump 42 again.
  • a heater (not shown) is disposed on the outer periphery of the piping members L4 and L5. Therefore, solidification of the organic EL element material in the piping members L4 and L5 can be prevented.
  • the material for organic EL element to be purified is a material used for the organic EL element and is not particularly limited.
  • known materials useful for purification by the purification apparatus of the present invention include, for example, N, N′-di- (naphthalen-1-yl) -N, N′-diphenyl-benzidine (NPB). Can be mentioned.
  • Step of liquefying solid organic EL element material First, the solid organic EL element material before purification is supplied to the hopper 34. Next, with the valve 31 c closed, the valve 31 a is opened, and a predetermined amount of solid organic EL element material is supplied into the liquefaction tank 31. After the supply, the valve 31a is closed, the valve 31c is opened, and the inside of the liquefaction tank 31 is depressurized to 10 ⁇ 1 Pa or less by the vacuum pump 36a. After decompression, the liquefaction tank 31 is heated by the infrared heater 35 to liquefy the solid organic EL element material. Heating by the infrared heater 35 is controlled by the temperature controller 8.
  • the inside of the supply tank 32 is depressurized, and the organic EL element material is removed from the supply tank 32 by the infrared heater 37. It heats to the temperature which does not solidify, and preparations for reception of a liquid organic EL element material are performed.
  • the valve 31b is opened, and the liquid organic EL element material is supplied into the supply tank 32. After replenishment, the valve 31b is closed and heating by the infrared heater 35 is stopped.
  • Step of supplying liquid organic EL element material to the apparatus body The step of supplying the liquid organic EL element material to the evaporator 6 of the apparatus main body 2 is performed as follows. After the liquefaction step or while the liquefaction step is being performed, preparation for receiving the liquid organic EL element material on the apparatus main body 2 side as described below is performed. First, with the discharge valve 44 and the valve 33b closed, the inside of the apparatus main body 2 is decompressed to 10 ⁇ 1 Pa or less by the vacuum pump 5. After decompression, the first cylinder 61 is heated by the heater 62, and the second cylinder 71 is heated by the temperature adjustment heater 72.
  • the temperature controller 8 controls heating by the heater 62 and the temperature adjusting heater 72 based on the measured temperature information of the temperature sensors 81 and 82.
  • the heater 62 heats the first cylinder 61 to a temperature at which the liquid organic EL element material evaporates (evaporation temperature), and maintains the temperature at the temperature.
  • the temperature adjustment heater 72 independently heats the first collection chamber 71A, the second collection chamber 71B, and the third collection chamber 71C to a predetermined temperature.
  • the first collection chamber 71A is heated and held higher than the temperature at which the organic EL element material to be purified condenses (condensation temperature), and the second collection chamber 71B is kept at the same temperature.
  • the third collection chamber 71C is heated and held at a lower temperature.
  • the valve 33a and the valve 33b are opened, the supply pump 33 is driven, and the liquid organic EL element material stored in the supply tank 32 is obtained. It supplies to the accommodating part 63.
  • the liquid organic EL element material reaches the nozzle 64 by the piping member L3 and is discharged into the accommodating portion 63 from the discharge port of the nozzle 64.
  • the supply amount to the evaporator 6 is controlled by the supply amount control means 3 ⁇ / b> C so that the liquid organic EL element material does not overflow or run out of the storage portion 63.
  • the temperature information detected by the liquid level detection sensor 39a (temperature sensors 391a, 392a, 393a) is transmitted to the valve controller 39b.
  • the valve controller 39b determines the liquid level of the liquid organic EL element material inside the container 63 based on the temperature information received from the liquid level detection sensor 39a. When it is determined that the liquid level has risen too much, the valve controller 39b reduces the supply amount by reducing the opening of the valve 33b, or closes the valve 33b and stops the supply pump 33. To stop the material supply. On the other hand, if it is determined that the liquid level has decreased, the valve controller 39b opens the valve 33b and operates the supply pump 33 if the supply is stopped, and the liquid organic EL element. Started supplying materials for use. If the supply amount is reduced by adjusting the opening degree of the valve 33b, the valve controller 39b increases the supply amount by increasing the opening degree of the valve 33b.
  • each collection chamber 71A, 71B, 71C is heated and held in the above-described relationship with respect to the condensation temperature of the organic EL element material to be purified. Therefore, the organic EL element material to be purified is collected with high purity in the second collection chamber 71B heated and held at the same temperature as the condensation temperature. In the first collection chamber 71A and the third collection chamber 71C, the impurity component contained in the liquid organic EL element material is concentrated and collected.
  • Step of recovering purified organic EL element material The organic EL element material purified in the purification step is recovered by the recovery device 4.
  • preparation for receiving the purified liquid organic EL element material on the collection device 4 side is performed as follows.
  • An empty collection container 41 with a clean interior is connected to the valve 42 a and the vacuum pump 43.
  • the valve 41 a is closed, the valve 41 b is opened, and the gas in the collection container 41 is once exhausted by the vacuum pump 43. After exhausting, the collection container 41 is filled with nitrogen.
  • the valve 41a, the valve 42a and the discharge valve 44 are opened, the transfer pump 42 is operated, and the liquid organic EL element material is placed in the collection container 41. to recover.
  • the discharge amount is controlled by the valve 41a, the transfer pump 42, the valve 42a and the discharge valve 44.
  • the valve 42b is closed.
  • the recovery container 41 is detached from the recovery device 4 with the valve 41a and the valve 41b being closed, and a separately prepared empty recovery container 41 is attached.
  • the collection is performed after the preparation for receiving on the collection device 4 side is performed as described above. At the time of attaching and removing the collection container 41, the above-described minimum flow line is formed, and the liquid organic EL element material is circulated.
  • Step of adding and liquefying liquid organic EL element material (additional liquefaction step)
  • the organic EL element material is added and liquefied.
  • the process to perform is implemented as follows.
  • the storage amount of the liquid organic EL element material in the supply tank 32 is controlled by the storage amount control means 38 and detected by the three liquid level detection sensors 38a (temperature sensors 381a, 382a, 383a).
  • the temperature information is transmitted to the storage amount controller 38b.
  • the storage amount controller 38b determines the liquid level of the liquid organic EL element material in the supply tank 32 based on the temperature information received from the liquid level detection sensor 38a.
  • the storage amount controller 38b displays the fact on the display means 38c. Based on this display, the decompression by the vacuum pump 36a is stopped, the valve 31c is closed, and the inside of the liquefaction tank 31 is returned to normal pressure. Thereafter, in the same manner as in the liquefaction step, the solid organic EL element material is liquefied and supplied into the supply tank 32.
  • the internal pressures of the liquefaction tank 31, the supply tank 32, the apparatus main body 2 and the recovery container 41 of the continuous liquefaction feeder 3 when the organic EL element material is continuously purified by the purification apparatus 1 are basically as follows. Adjusted to a good relationship. (Liquefaction tank 31)> (Supply tank 32)> (Device main body 2)> (Recovery container 41) Without using the supply pump 33 and the transfer pump 42, the supply from the liquefaction tank 31 to the supply tank 32, the supply from the supply tank 32 to the apparatus main body 2, and the recovery from the apparatus main body 2 to the collection container 41 are each performed as liquid. In the case where the self-weight of the organic EL element material is used, each internal pressure is adjusted in this order.
  • the liquefied continuous supply device 3 continuously supplies the solid organic EL element material into a liquid state and then continuously supplies the material to the accommodating portion 63 in the evaporator 6. Therefore, it is not necessary to perform batch processing for heating and cooling the apparatus for every predetermined amount of purification as in the conventional purification apparatus, and the purification can be performed continuously. Therefore, according to the refiner
  • the valve controller 39b determines the remaining amount of the organic EL element material in the storage unit 63 based on the temperature information detected by the liquid level detection sensor 39a.
  • the valve controller 39b controls the supply pump 33 and the valve 33b based on the determination result. Therefore, even if the purification is continuously performed, it is possible to prevent the liquid organic EL element material in the storage unit 63 from being lost or overflowing from the storage unit 63. Therefore, according to the refiner
  • the storage amount controller 38 b determines the storage amount of the liquid organic EL element material in the supply tank 32 based on the temperature information detected by the liquid level detection sensor 38 a of the storage amount control means 38.
  • the solid organic EL element material can be liquefied in the liquefaction tank 31 based on the determination result and supplied to the supply tank 32. That is, the liquid organic EL element material in the supply tank 32 can be maintained at a predetermined amount or more. Therefore, according to the refiner
  • the collection containers 41 of the collection apparatuses 4A, 4B, and 4C are detachably connected to the discharge holes 73a of the collection chambers 71A, 71B, and 71C. Therefore, even if the organic EL element material is continuously purified and the collected organic EL element material is increased, it can be recovered in the recovery container 41 outside the apparatus main body 2 for recovery. There is no need to stop purification. Further, since the collection container 41 is detachably connected, when the collection container 41 is filled with the purified organic EL element material, only the collection is temporarily stopped and replaced with another collection container 41. be able to. Therefore, according to the refining device 1, since it is not necessary to stop the refining when collecting the purified organic EL element material, the continuous purification of the organic EL element material can be performed more stably.
  • the collector 7 has three collection chambers 71A, 71B, and 71C having different temperatures continuously or stepwise. Therefore, it is possible to accurately classify a collection chamber in which high-purity organic EL element materials are collected and a collection chamber in which more impurities are collected. And since each collection chamber 71A, 71B, 71C is connected to the collection container 41 for the organic EL element material that has been liquefied and collected, impurities compared with the high purity organic EL element material The organic EL element material containing a large amount of can be accurately sorted and collected. Therefore, according to the refiner
  • the refining device 1 since heaters are arranged on the outer periphery of the piping members L2, L3, L4, and L5 through which the liquid organic EL element material passes, the inside of the piping members L2, L3, L4, and L5 Solidification of the organic EL element material can be prevented. Therefore, according to the refiner
  • a minimum flow line is formed in the recovery apparatus 4. Therefore, when the collection container 41 is attached and removed, the liquid organic EL element material can be circulated through the minimum flow line, so that the solidification of the organic EL element material can be prevented. Therefore, according to the refiner
  • the refining device 1 is provided with shielding portions 23 on the upstream side and the downstream side of the device body 2. Therefore, a temperature drop inside the apparatus main body 2 can be prevented. Further, the gaseous organic EL element material moves to and adheres to the upstream lid portion 21 or passes through the third collection chamber 71C and further moves to and adheres to the downstream lid portion 22. Can be prevented. As a result, the organic EL element material supplied to the evaporator 6 can be more reliably collected in each of the collection chambers 71A, 71B, 71C, and the amount of material loss can be reduced.
  • FIG. 5 shows a schematic cross-sectional view of the purification apparatus 1A.
  • the purification apparatus 1A and the purification apparatus 1 of the first embodiment differ in the structure of the apparatus main body.
  • the apparatus main body 2A of the second embodiment has a double tube structure in which a cylindrical outer tube 210 and a cylindrical inner tube 220 are arranged inside the outer tube 210, whereas the apparatus main body 2A is a first tube.
  • the apparatus main body 2 is different in that it has a single-pipe structure.
  • the purification apparatus 1A includes an apparatus body 2A for purifying the organic EL element material, a liquefied continuous supply device 3 for supplying the organic EL element material to the apparatus body 2A, A recovery device 4 that recovers the later organic EL element material, a vacuum pump 5 that depressurizes the interior of the apparatus main body 2A, and a temperature controller 8 that controls the temperature of the apparatus main body 2 are provided.
  • the supply of the organic EL element material is controlled by the supply amount control means 3C as in the first embodiment.
  • the evaporator 6A is disposed on the upstream side of the apparatus main body 2A, and the collector 7A is disposed on the downstream side of the apparatus main body 2A, as in the purification apparatus 1 of the first embodiment.
  • the evaporator 6A includes a cylindrical first cylinder 65.
  • the first cylinder 65 is arranged on the upstream side of the inner cylinder 220, and the accommodating portion 63, the nozzle 64, and the temperature sensor 81 are arranged inside the first cylinder 65.
  • the liquid organic EL element material evaporates inside the first cylinder 65.
  • the 1st cylinder 65 is comprised with a material inactive with respect to an organic EL element material.
  • flange portions 66 projecting inward in the radial direction of the cylinder are formed.
  • this flange portion 66 prevented unpurified organic EL element material from flowing into the collector 7A, and was further collected by the collector 7A.
  • the organic EL element material is prevented from flowing into the evaporator 6A side.
  • the flange portion 66 is used for connection with the second cylinder 75 and the shielding plate 231 of the collector 7A as described later.
  • a heater 62 is disposed so as to surround the outer periphery of the outer tube 210.
  • the collector 7 ⁇ / b> A includes a cylindrical second cylinder 75.
  • the second cylinder 75 is formed by connecting a plurality of cylindrical collection cylinders.
  • three collection cylinders that is, the first collection cylinder 75A, the second collection cylinder 75B, and the third collection cylinder 75C are connected in order from the upstream side.
  • the insides of the collection cylinders 75A, 75B, and 75C correspond to the collection chambers 71A, 71B, and 71C in the first embodiment, respectively.
  • the 2nd cylinder 75 is comprised with a material inactive with respect to an organic EL element material.
  • a temperature sensor 82 is disposed inside each collection cylinder 75A, 75B, 75C.
  • the liquid organic EL element material is condensed and collected on the inner surfaces of the collection cylinders 75A, 75B, and 75C.
  • a quartz tube 73 is connected to each of the collecting cylinders 75A, 75B, and 75C, and a discharge hole 73a is formed.
  • the inclined surface 74 is formed in the lower inner surface of each collection cylinder 75A, 75B, 75C similarly to 1st embodiment.
  • a temperature adjusting heater 72 is arranged so as to surround the outer periphery of the outer tube 210.
  • Flange portions 76 projecting inward in the radial direction of the cylinder are formed at both ends of each collection cylinder 75A, 75B, 75C.
  • the flange portion 76 has a collection chamber in which the purified organic EL element materials collected by the collection cylinders 75A, 75B, and 75C are adjacent to each other. It is prevented from flowing into the single cylinder 65 or the lid portion 22.
  • the flange part 76 is utilized when connecting each collection cylinder 75A, 75B, 75C so that attachment or detachment is possible.
  • a through-hole is formed in the flange portion 76, a connecting member such as a bolt is inserted into both flange portions 76 of adjacent collecting cylinders, and the collecting cylinders are connected by a fixing member such as a nut. Secure. Furthermore, when connecting the above-mentioned 1st cylinder 65 and the 2nd cylinder 75 so that attachment or detachment is possible, the flange part 66 of the 1st cylinder 65 is utilized. A through-hole is formed in the flange portion 66 in the same manner as the flange portion 76, and is connected to the flange portion 76 of the first collection cylinder 75A by a connecting member and a fixing member.
  • the inner cylinder pipe 220 is comprised by the 1st cylinder 65 and the 2nd cylinder 75 being connected by the axial direction of a cylinder.
  • the outer tube 210 is formed so that the inner tube 220 can be detachably accommodated therein, and the material is preferably made of a material that is inactive with respect to the organic EL element material. Then, it consists of quartz glass. Three quartz tubes 211 for discharging the collected liquid organic EL element material to the outside are connected to the outer tube 210, and the collected organic EL element material is discharged inside the quartz tube 211. The discharge hole 211a for this purpose. The connection positions of the three quartz tubes 211 correspond to the positions of the three quartz tubes 73 of the collection cylinders 75A, 75B, and 75C arranged inside the outer tube 210.
  • the quartz tube 211 and the quartz tube 73 are detachably connected via a seal member 212 such as packing, and leakage of the liquid organic EL element material from the connection portion is prevented. Further, when the quartz tube 211 and the quartz tube 73 are connected, the discharge hole 211a and the discharge hole 73a communicate with each other, and the collected liquid organic EL element material becomes the discharge hole 73a and the discharge hole. It is discharged outside the apparatus main body 2A through 211a.
  • two shielding portions 23 are formed on each of the upstream side and the downstream side of the apparatus main body 2A.
  • the diameter of the shielding plate 231 is formed to be larger than the inner diameters of the cylinders of the first cylinder 65 and the second cylinder 75 and slightly smaller than the inner diameter of the outer tube 210, and the inner surface of the apparatus main body 2 and the shielding plate 231. It is formed so that no gap is formed between the side surfaces. It is preferable to connect the innermost shielding plate 231 of the apparatus main body 2 ⁇ / b> A to the end of the inner tube 220.
  • the through hole as described above is formed in the flange portion 66 of the first cylinder 65 or the flange portion 76 of the second cylinder 75, and the through hole and the through hole 232 of the shielding plate 231 are formed.
  • Use and connect By connecting in this way, the openings on both ends of the inner tube 220 are shielded by the shielding part 23, so that the gaseous organic EL element material is used for the first tube 65 and the second tube during purification. It is possible to prevent leakage to the outside of 75.
  • the organic EL element material can be purified in the same manner as in the first embodiment.
  • the apparatus main body 2A of the second embodiment includes an outer tube 210 and an inner tube 220, and the inner tube 220 is detachably accommodated inside the outer tube 210.
  • the organic EL element material adheres mainly to the inner surfaces of the first cylinder 65 and the second cylinder 75 constituting the inner cylinder 220.
  • the inner surface of the outer tube 210 is less likely to adhere to the organic EL element material, so that cleaning is easy.
  • the inner tube 220 can be taken out from the outer tube 210, the first tube 65 and the second tube 75 can be easily cleaned. Further, since the double tube structure is used as in the apparatus main body 2A, during the cleaning by removing the inner tube 220, another inner tube 220 can be placed in the outer tube 210 and the purification can be started. Therefore, the operation rate of the purification apparatus 1A can be increased.
  • the flange portion 66 of the first cylinder 65 and the flange portion 76 of the second cylinder 75 protrude toward the radially inner side of the cylinder.
  • it functions in the same manner as the weir plates 68 and 78 described in the first embodiment, and the condensed organic EL element material is mixed between the adjacent cylinders 65 and 75 (75A, 75B, and 75C). Can be prevented.
  • FIG. 6 shows a schematic cross-sectional view of the purification apparatus 1B.
  • the purification apparatus 1B and the purification apparatus 1 of the first embodiment mainly differ in the mounting angle of the apparatus main body.
  • the apparatus main body 2B of the third embodiment is formed in a cylindrical shape and is placed with its axial direction inclined with respect to the horizontal direction, whereas the apparatus main body 2 of the first embodiment is cylindrical. It differs in that it is placed so that the axial direction is substantially along the horizontal direction.
  • the apparatus main body 2B is inclined at an angle ⁇ with respect to the horizontal plane by placing the apparatus so that the downstream side is higher than the upstream side of the apparatus main body 2B.
  • the position of the discharge hole 73a differs between the purification apparatus 1B and the purification apparatus 1.
  • the position of the discharge hole 73a of the apparatus main body 2B is close to the upstream side of each of the collection chambers 71A, 71B, 71C. Points other than those described above are configured similarly in the purification apparatus 1B and the purification apparatus 1 and can be purified by the same purification method, and thus the description thereof is omitted.
  • the apparatus main body 2B of 3rd embodiment is mounted so that a downstream side may become higher than the upstream of the apparatus main body 2B, like the refiner
  • the downstream side may be placed lower.
  • the dam plate 78 is located on the downstream side of the discharge hole 73a of the apparatus main body 2B, and the discharge hole 73a is formed on the upstream side of the dam plate 78. That is, the position of the discharge hole 73a is formed at the upstream end of the collection chambers 71A, 71B, 71C in the case of the purification apparatus 1B shown in FIG. 6, whereas the purification apparatus 1C shown in FIG. In this case, it is formed at the downstream end of each of the collection chambers 71A, 71B, 71C.
  • the device main body 2B is placed so that the downstream side is elevated, and is inclined at an angle ⁇ with respect to the horizontal plane. Since the position of the discharge hole 73a is closer to the upstream side, the discharge hole 73a is formed at a low position in each of the collection chambers 71A, 71B, 71C. Therefore, since the organic EL element material condensed in the collector 7 is easily collected in the discharge hole 73a, the purified organic EL element material can be collected more rapidly.
  • the liquid level detection sensor 38 a may be configured to visually confirm the liquid level using a level gauge 384.
  • a level detector such as a float type, an ultrasonic type, a capacitance type, a pressure type, or an optical type can be applied.
  • the liquid level detection sensor 39a may be configured to detect the liquid level using a level detector 394.
  • a detection method a float type, a capacitance type, a pressure type An optical type or the like can be applied.
  • a flow meter 33c is provided on the discharge side of the valve 33b, and the supply amount of the liquid organic EL element material to the accommodating portion 63 is controlled based on the measurement value of the flow meter 33c. It is good also as a structure to perform.
  • the relationship between the pump stroke of the supply pump 33 and the flow rate when the organic EL element material is circulated may be grasped in advance, and the supply amount may be controlled by adjusting the pump stroke.
  • the supply amount may be controlled by a method. Further, the liquid level detection by the liquid level detection sensor 39a and the control by the flow meter 33c and the pump stroke of the supply pump 33 may be combined to control the supply pump 33 and the valve 33b by the valve controller 39b. good.
  • the shape of the apparatus main body of the present invention is not particularly limited.
  • the case where the apparatus main body is cylindrical has been described as an example.
  • an arbitrary shape such as a box shape, a cylindrical shape, a tank shape, a cubic shape, and the like can be given.
  • examples of the cross-sectional shape of the apparatus main body include a circular shape, a quadrangular shape, and a semicircular shape.
  • the cross-sectional shape may be constant in the apparatus main body, or the cross-sectional shape may be partially different.
  • the outer tube and the inner tube may not have the same cross-sectional shape.
  • quartz glass is mainly described as an inactive material with respect to the organic EL element material.
  • the present invention is not limited to this. Examples include stainless steel, tantalum, tungsten, molybdenum, titanium, zirconia, carbon, alumina, boron nitride, silicon nitride, and Teflon (registered trademark).
  • the material of the apparatus main body is not limited to the case where the whole is an inactive material with respect to the organic EL element material. It can also be comprised with the said inert material about the site
  • the organic EL element material supplied from the liquefied continuous supply device to the evaporator has been described as an example of being stored in the storage portion, but is not limited thereto. You may supply to the inside of the 1st cylinder of an evaporator not via an accommodating part.
  • the heating means and heating method for heating the evaporator and the collector are not limited to those described in the above embodiment.
  • the heating method resistance heating method (metal type, non-metal type, etc.), light heating method (infrared heating method, arc radiation heating, laser radiation heating, etc.), induction heating method, plasma heating method, arc heating method, flame heating The law etc. can be mentioned.
  • the evaporator and the collector are made of a material that generates heat by electromagnetic induction, such as stainless steel.
  • the present invention is not limited to this. Although it depends on the size of the apparatus main body, it is easy to obtain a higher-purity organic EL element material by increasing the number of collection chambers and collecting at a higher temperature setting. Similarly, in the second embodiment, the number of collecting cylinders constituting the second cylinder of the collector is not limited to three.
  • the barrier plate formed on the first cylinder or the second cylinder may be formed integrally with the first cylinder or the second cylinder, or may be formed separately.
  • the setting of the heating temperature for each collection chamber of the collector is not limited to that described in the above embodiment.
  • a minimum flow line similar to that provided in the recovery device may be formed in the supply amount control means.
  • a branch point is provided between the supply pump 33 and the valve 33b
  • a junction point is provided between the supply pump 33 and the valve 33a
  • the junction point and the junction point are connected by a piping member via the valve. .
  • the recovery apparatus has been described by taking the aspect of using the recovery pump as an example, but the present invention is not limited to this.
  • the recovery device 4 may be disposed at a position lower than the purification device main body so as to flow into the recovery container using the weight of the liquid organic EL element material itself without using the recovery pump. good.
  • the present invention is not limited thereto, and for example, the upstream side and the downstream side of the apparatus main body 2 It is good also as a structure which provided one each in each.
  • the said embodiment gave and demonstrated the example which comprised the some circular shielding board connected about the shielding part, it is not limited to this. For example, you may comprise a shielding part with one shielding board.
  • a shielding plate may be provided close to the upstream side of the accommodating portion 63 inside the first cylinder 65.
  • the organic EL element material does not flow to the upstream side but flows to the downstream side, so the organic EL element material is collected more efficiently. become able to.
  • the temperature fall inside the 1st cylinder 65 can be suppressed.
  • a shielding plate may be attached to the downstream end portion of the second cylinder 75 (third collection cylinder 75C). As a result, the organic EL element material is prevented from being discharged from the downstream end of the second cylinder 75 to the outside of the apparatus main body 2 or the decrease in the internal temperature of the second cylinder 75 is suppressed. be able to.
  • the organic material purified by the purification apparatus of the present invention is not limited to the organic EL element material. Moreover, the organic material refine
  • the present invention can be used for refining organic materials such as materials for organic EL elements.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Electroluminescent Light Sources (AREA)

Abstract

L'invention concerne un appareil de purification (1) qui est caractérisé comme comportant : un évaporateur (6) qui est doté d'un premier corps cylindrique (61), dans lequel une matière organique est introduite, et d'un dispositif de chauffage chauffant (62) qui est disposé à l'extérieur du premier corps cylindrique (61) et fait évaporer la matière organique introduite ; un collecteur (7) qui est doté d'un second corps cylindrique (71) qui communique avec le premier corps cylindrique (61) de l'évaporateur (6) et d'un dispositif de chauffage et de régulation de température (72) qui est disposé à l'extérieur du second corps cylindrique (71) et régule la température du second corps cylindrique (71), ledit collecteur (7) collectant la matière organique qui a été évaporée par l'évaporateur (6) et dans un état gazeux, par liquéfaction de la matière organique gazeuse sur la surface interne du second corps cylindrique (71) ; et une unité d'alimentation en continu de liquéfaction (3) qui liquéfie la matière organique à l'état solide et fournit en continu la matière organique dans un état liquide dans l'évaporateur (6).
PCT/JP2012/077852 2011-10-31 2012-10-29 Appareil de purification d'une matière organique et procédé de purification d'une matière organique WO2013065626A1 (fr)

Priority Applications (1)

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KR1020147012663A KR20140084165A (ko) 2011-10-31 2012-10-29 유기 재료의 정제 장치 및 유기 재료의 정제 방법

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JP2011-239354 2011-10-31
JP2011239354 2011-10-31
JP2012-083212 2012-03-30
JP2012083212A JP2013116879A (ja) 2011-10-31 2012-03-30 有機材料の精製装置及び有機材料の精製方法

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WO2013065626A1 true WO2013065626A1 (fr) 2013-05-10

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WO2016008312A1 (fr) * 2014-07-15 2016-01-21 广东阿格蕾雅光电材料有限公司 Nouvelle méthode de purification de matériau organique solide
CN109923689A (zh) * 2017-09-20 2019-06-21 株式会社Lg化学 作为有机发光元件的材料使用的有机物质的纯化方法
TWI833735B (zh) * 2018-02-28 2024-03-01 美商蘭姆研究公司 用於高對流連續旋轉鍍覆之流輔助動態封件

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KR101547096B1 (ko) 2015-01-27 2015-08-24 한국생산기술연구원 이온성 액체를 이용한 유기소재 정제방법 및 정제장치
CN106030847B (zh) 2014-02-14 2018-12-11 伊尔索勒德株式会社 利用离子性液体的有机材料提纯方法及提纯装置
CN105291325A (zh) * 2014-07-11 2016-02-03 广东阿格蕾雅光电材料有限公司 有机固体材料连续蒸馏浇注成型装置
CN105311852A (zh) * 2014-07-15 2016-02-10 广东阿格蕾雅光电材料有限公司 有机固体材料连续蒸馏装置
JP2019111507A (ja) * 2017-12-26 2019-07-11 株式会社 エイエルエステクノロジー 精製装置
KR102073740B1 (ko) * 2018-04-30 2020-02-05 고려대학교 산학협력단 연속식 유기물 진공증발정제장치
KR20200123894A (ko) 2019-04-22 2020-11-02 (주)일솔레드 이온성 액체를 이용한 유기소재의 기액용해 재결정화 방법 및 장치
KR20200126460A (ko) 2019-04-29 2020-11-09 (주)일솔레드 유기소재 인라인 정제 시스템
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WO2016008312A1 (fr) * 2014-07-15 2016-01-21 广东阿格蕾雅光电材料有限公司 Nouvelle méthode de purification de matériau organique solide
CN109923689A (zh) * 2017-09-20 2019-06-21 株式会社Lg化学 作为有机发光元件的材料使用的有机物质的纯化方法
CN109923689B (zh) * 2017-09-20 2020-06-19 株式会社Lg化学 作为有机发光元件的材料使用的有机物质的纯化方法
TWI833735B (zh) * 2018-02-28 2024-03-01 美商蘭姆研究公司 用於高對流連續旋轉鍍覆之流輔助動態封件

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