JP6006516B2 - Organic material purification equipment - Google Patents

Description

  The present invention relates to an organic material purification apparatus.

Conventionally, column chromatography, recrystallization, distillation, sublimation and the like are known as methods for purifying organic materials. An 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.
As an example of an electronic material, a material used for an organic electroluminescence element (hereinafter sometimes referred to as an organic EL element) which has been actively researched and developed in recent years can be given. If impurities are mixed in a material used for an organic EL element (hereinafter sometimes referred to as a material for an organic EL element), the impurity becomes a trap of carriers (electrons and holes) or quenches. Cause the emission intensity, emission efficiency, and durability of the organic EL element to decrease. Therefore, in order to reduce impurities, it is necessary to purify the organic EL element material with high purity.

  As a refinement | purification apparatus for refine | purifying an organic EL element material, it is disclosed by patent document 1, for example. The refining device described in Patent Literature 1 includes an inner pipe divided into a plurality of sections by a connecting member having a partition wall and a hole provided in the approximate center thereof, and is configured to be able to control the temperature of each section. . And in the refinement | purification apparatus described in patent document 1, a vacuum pump is arrange | positioned at the end of an inner tube, and carrier gas is supplied from the other side (other end) of an inner tube. A cell holding the substance to be purified (organic electroluminescent material) is placed in the first section of the inner tube, the inside of the apparatus is depressurized with a vacuum pump, the carrier gas flows, and the first section is heated. Then, the substance to be purified is sublimated. Impurities of the sublimated purification target substance are prevented from moving to other sections by the partition walls and holes, and the purification target substance gradually passes through the holes of the partition walls and moves to the other sections. Purified.

  Moreover, in the refinement | purification apparatus described in patent document 2, the disk-shaped rectification | straightening board arrange | positioned so that an opening part may not mutually overlap in an axial direction is provided in the inner cylinder body where the sublimated organic material distribute | circulates in several places. Yes. The organic material flows through this opening while bending, and adheres to the inner peripheral surface of the inner cylinder and the front and back surfaces of the current plate. Further, the rectifying plate prevents the downstream impurities from flowing backward.

JP 2005-511864 A JP 2011-50853 A

In the refining device described in Patent Document 1, each section is divided by a connecting member having a hole provided substantially at the center, but the organic electroluminescent material that circulates in the central portion of the inner tube cross section is formed on the inner surface of the inner tube. Without contact, there is a risk of passing through the hole to the downstream side and being discharged out of the apparatus. As a result, the organic material is not collected but sucked into the vacuum pump, the amount of purification of the desired organic material is reduced, and the purification efficiency is lowered. In particular, when the diameter of the inner tube is increased in order to increase the amount of purification of the organic material, the organic electroluminescent material is likely to flow through the center of the cross section of the second cylinder, and the purification efficiency is reduced.
Further, in the purification apparatus described in Patent Document 2, since the disc-shaped rectifying plate is provided in a plurality of locations in the axial direction inside the inner cylindrical body, the organic material that circulates in the center of the cross section of the inner cylindrical body is also Touch the current plate. However, in the refining device described in Patent Document 2, it is necessary to provide a large number of rectifying plates for the purpose of preventing the downstream impurities from flowing back, and as a result, the organic material frequently flows to the downstream side while meandering. As a result, the purification takes time and the purification efficiency decreases.

  The objective of this invention is providing the refiner | purifier of the organic material which can improve the refinement | purification efficiency of an organic material.

The organic material refining device of the present invention comprises:
A vaporizer including a first cylinder to which an organic material is supplied, and a heater disposed on the outside of the first cylinder to vaporize the supplied organic material;
A second cylinder communicating with the first cylinder of the vaporizer; and a temperature adjusting heater disposed outside the second cylinder for adjusting the temperature of the second cylinder; vaporizing by the vaporizer A collector for collecting the gaseous organic material on the inner surface of the second cylinder;
A collection area expanding member disposed inside the second cylinder, having a surface extending along the axial direction of the second cylinder, and increasing a contact area with the gaseous organic material;
And an exhaust device connected to the downstream end of the collector.

According to this invention, the collection area expansion member which has a surface extended along the axial direction of the said 2nd cylinder inside the 2nd cylinder is arrange | positioned. An exhaust device is connected to the downstream end of the collector. Therefore, an air flow from the inside of the first cylinder to the inside of the second cylinder is generated by the exhaust device, and the gaseous organic material comes into contact with the inner surface of the second cylinder and the surface of the collection area expanding member, and is solidified or liquefied. To be collected. In other words, the collection area expanding member enlarges the area of the collection surface where the organic material is collected, and increases the number of sites where the organic material flowing through the central portion of the cross section of the second cylindrical body comes into contact, thereby facilitating collection. It is a member.
Further, according to the present invention, the organic material is formed between the inner surface of the second cylinder and the surface of the collection area enlarging member and flows through the flow path extending in the axial direction of the second cylinder, so that the exhaust gas is exhausted. There is little resistance, and the organic material can be efficiently circulated downstream in a short time.
Therefore, according to the present invention, the organic material can be collected not only on the inner surface of the second cylinder but also on the surface of the collection area expanding member, and the purification efficiency of the organic material can be improved.

  In the organic material refining device according to the present invention, it is preferable that the collection area enlarging member is disposed at the center of the cross section of the second cylinder.

  According to this invention, the collection area expansion member is arrange | positioned in the cross-sectional center part of the 2nd cylinder. Therefore, the organic material which is going to distribute | circulate the said cross-sectional center part comes in contact with a collection area expansion member, or comes closer to the inner surface of a 2nd cylinder body avoiding a collection area expansion member, and distribute | circulates. As a result, the organic material easily comes into contact with the inner surface of the second cylindrical body and the surface of the collection area expanding member. Therefore, according to the present invention, the purification efficiency of the organic material can be improved.

In the organic material purification apparatus of the present invention,
The collection area expanding member is a cylindrical third cylinder,
The axial direction of the third cylinder is preferably along the axial direction of the second cylinder.

According to the present invention, the third cylinder is disposed along the axial direction of the second cylinder. Since the organic material can contact the inner surface of the second cylinder, the inner surface of the third cylinder, and the outer surface, the contact area increases.
Therefore, according to the present invention, the purification efficiency of the organic material can be further improved.

  In the organic material refining device of the present invention, it is preferable that the openings at both ends of the third cylinder are sealed.

According to the present invention, since the openings at both ends of the third cylinder are sealed, the space inside the second cylinder through which the organic material can circulate can be reduced. And the airflow which goes to the inside of a 2nd cylinder from the inside of a 1st cylinder does not pass the inside of a 3rd cylinder, but comes to pass between the 2nd cylinder inner surface and a 3rd cylinder outer surface. Therefore, according to the present invention, the organic material can be efficiently collected on the inner surface of the second cylinder and the outer surface of the third cylinder, and the purification efficiency can be further improved.
In addition, according to the present invention, since the organic material is selectively collected on the inner surface of the second cylinder and the outer surface of the third cylinder, the recovery operation after purification is facilitated.

  In the organic material refining device of the present invention, it is preferable that a plurality of ribs extending in the axial direction of the third cylinder are provided on the outer surface of the third cylinder.

  According to this invention, the some rib extended over the axial direction of a 3rd cylinder is provided in the outer surface of the 3rd cylinder. Therefore, according to the present invention, the organic material channel formed between the inner surface of the second cylinder and the outer surface of the third cylinder can be divided into a plurality of smaller channels extending in the axial direction. That is, a divided flow path can be formed. As a result, the organic material is collected on the inner surface of the second cylinder, the outer surface of the third cylinder, and the rib surface while passing through the divided flow path. Therefore, according to the present invention, the purification efficiency of the organic material can be further improved.

  In the organic material refining device according to the present invention, the plurality of ribs protrude from the outer surface of the third cylinder toward the inner surface of the second cylinder, from the upstream side to the downstream side of the third cylinder. It is preferable that they are provided differently on the way to.

  According to the present invention, the plurality of ribs are provided such that the direction in which the rib protrudes from the outer surface of the third cylinder toward the inner surface of the second cylinder is different in the middle from the upstream side to the downstream side of the third cylinder. Therefore, the divided flow path can be meandered. As a result, since the organic material flows toward the downstream side while meandering through the divided flow path, the organic material is further easily collected on the second cylinder inner surface, the third cylinder outer surface, and the rib surface. Therefore, according to the present invention, the purification efficiency of the organic material can be further improved.

  In the organic material refining device of the present invention, the collection area expanding member may be a lattice member formed in a lattice shape by combining a plurality of plate-like members extending along the axial direction of the second cylindrical body. preferable.

  According to the present invention, the collection area enlarging member is a lattice member formed in a lattice shape by combining a plurality of plate-like members extending along the axial direction of the second cylindrical body, so that more divided flow paths are provided. Can be formed. Therefore, according to the present invention, the organic EL element material can be collected not only on the inner surface of the second inner cylinder but also on the surface of the lattice member, and the purification efficiency can be improved.

  In the organic material refining device of the present invention, the collection area expanding member is preferably formed to be separable.

  According to this invention, the said collection area expansion member is formed so that division | segmentation is possible. Therefore, according to the present invention, the organic material can be collected more easily than in the case where the collection surface of the organic material remains a cylinder or a lattice member.

  In the organic material refining device of the present invention, it is preferable that the second cylinder is formed to be separable.

  According to this invention, the 2nd cylinder is formed so that division | segmentation is possible. Therefore, according to this invention, compared with the case where the collection surface of an organic material remains a cylinder, collection | recovery of an organic material becomes easy.

  In the organic material refining device of the present invention, it is preferable that the second cylinder and the third cylinder are formed of an inert metal or ceramics.

  According to the present invention, an inert metal or ceramics can be used as the material of the second cylinder and the third cylinder. Therefore, it becomes possible to select a material suitable for the refining work of the organic material, and the refining work becomes easy. Examples of the inert metal include stainless steel, tantalum, tungsten, molybdenum, and titanium. Examples of the ceramic include quartz, zirconia, alumina, boron nitride, and silicon nitride. For example, if it is made of stainless steel, the second cylinder and the third cylinder can be prevented from being damaged. Further, if made of quartz, quartz has low stretchability, and the inside can be easily confirmed.

In the organic material purification apparatus of the present invention,
An outer cylinder that houses the first cylinder and the second cylinder;
The heater is disposed outside the first cylinder and the outer cylinder,
The temperature adjusting heater is preferably disposed outside the second cylinder and the outer cylinder.

According to the present invention, the refining device has a double tube structure in which the first tube and the second tube are accommodated inside the outer tube, and the refining device in such a double tube structure is being refined. Even so, the internal temperature of the second cylinder can be measured and controlled more accurately. Therefore, according to the present invention, not only the inner surface of the second cylindrical body but also the surface of the collection area expanding member can be collected in the purification apparatus having a double-pipe structure, and the purification efficiency of the organic material can be improved. Can be improved.
In addition, since the refining device has a double-pipe structure, the first and second cylinders are removed from the outside of the apparatus and cleaned while the other first and second cylinders are removed from the outer cylinder. Place it inside the body and start purification. Therefore, the operating rate of the refiner can be improved.

It is a section schematic diagram of the refining device of the organic material concerning a first embodiment of the present invention. It is a section schematic diagram of the vaporizer of the refining device concerning the first embodiment. It is a section schematic diagram of a collector of a refining device concerning the first embodiment. FIG. 4 is a schematic cross-sectional view of the collector of the purification apparatus according to the first embodiment, and is a view on the downstream side of the cross-sectional position of FIG. 3. It is a perspective view of the collection cylinder which comprises the 2nd cylinder of the said collector. It is a perspective view of the collection cylinder different from FIG. 5 which comprises the 2nd cylinder of the said collector. It is a perspective view of the sealing cylinder attached to the upstream edge part of the said collector. It is a perspective view of the 2nd cylinder concerning a second embodiment. It is a perspective view of the 3rd cylinder concerning the second embodiment. It is the cross-sectional schematic of the refiner | purifier of the organic material which concerns on 3rd embodiment. It is a section schematic diagram of a collector of a refining device concerning the third embodiment. It is a perspective view explaining the shape of the collection area expansion member which concerns on the modification of embodiment. It is sectional drawing explaining the shape of the said collection area expansion member which concerns on the modification of embodiment. It is sectional drawing explaining the shape of another collection area expansion member which concerns on the modification of embodiment.

  Hereinafter, embodiments of the present invention will be described with reference to the drawings.

<First embodiment>
(1) Structure of refiner | purifier The schematic of the cross section along the longitudinal direction of the refiner | purifier 1 of the organic material which concerns on 1st embodiment is shown by FIG.
The purification device 1 includes a device main body 2 for purifying an organic material, a vacuum pump 3 as an exhaust device for reducing the pressure inside the device main body 2, and a temperature controller 4 for controlling the temperature of the device main body 2. Hereinafter, the case where an organic EL element material is purified will be described as an example.

(1-1) Device Main Body The device main body 2 includes a cylindrical inner cylinder 21 and a cylindrical outer cylinder 22 that is disposed outside the inner cylinder 21 and accommodates the inner cylinder 21 therein. And a double pipe structure in which both ends of the outer cylinder body 22 are closed by the lid portions 23 and 24.
The apparatus main body 2 is provided with a vaporizer 5 on one side of the inner cylinder body 21 and the outer cylinder body 22, and a collector 6 is provided on the other side of the inner cylinder body 21 and the outer cylinder body 22. The container 5 and the collector 6 are provided continuously in the horizontal direction of the apparatus main body 2.
Moreover, as shown in FIG. 1, the vacuum pump 3 is connected to the cover part 24 provided in the edge part by the side of the collector 6 of the apparatus main body 2. As shown in FIG. The vacuum pump 3 is provided with a piping member via a valve 3 a, and the piping member is connected to the lid portion 24 so as to communicate with the inside of the apparatus main body 2. Therefore, the vacuum pump 3 can exhaust the inside of the apparatus main body 2. In this embodiment, the pressure in the apparatus main body 2 is set to 10 ⁻¹ Pa or less. It is preferable that a trap device (not shown) is interposed between the apparatus main body 2 and the vacuum pump 3.

  In such an apparatus main body 2, the organic EL element material is vaporized inside the vaporizer 5, and the vaporized gaseous organic EL element material flows into the collector 6 by suction of the vacuum pump 3 and is collected. It is solidified and collected inside the collector 6. Thus, the organic EL element material to be purified flows from the vaporizer 5 side to the collector 6 side. Hereinafter, in accordance with the flow direction of the organic EL element material, one side where the vaporizer 5 of the apparatus main body 2 is arranged is upstream, and the other side where the collector 6 of the apparatus main body 2 is arranged downstream. Sometimes referred to as the side.

(1-1-1) Vaporizer The vaporizer 5 is disposed on the upstream side of the apparatus main body 2. The vaporizer 5 constitutes a first inner cylinder 51 as a first cylinder constituting the upstream side of the inner cylinder 21, and an upstream side of the outer cylinder 22, and is disposed outside the first inner cylinder 51. A first outer cylindrical body 52, a heater 53 disposed outside the first outer cylindrical body 52, and an accommodating portion 54 as a raw material container disposed inside the first inner cylindrical body 51.

FIG. 2 shows a cross-sectional view of the first inner cylinder 51 and the first outer cylinder 52 of the vaporizer 5.
The first inner cylinder 51 and the first outer cylinder 52 are formed in a cylindrical shape.
On the inner surface of the first inner cylinder 51, support protrusions 512 for supporting the accommodating portion 54 are formed on the left and right as shown in FIG.

The heater 53 is configured by an infrared heater or the like, and is arranged in an annular shape outside the first outer cylinder 52.
The accommodating portion 54 is disposed inside the first inner cylindrical body 51. The accommodating portion 54 is formed in a dish shape having, for example, a rectangular plate-shaped bottom surface and a side surface rising from the periphery of the bottom surface in the out-of-plane direction, and accommodates solid organic EL element materials such as powder. Yes.
The material of the first inner cylinder 51, the first outer cylinder 52, and the housing portion 54 is preferably made of a material that is inert with respect to the organic EL element material. In the present embodiment, the material is quartz glass. It is configured.

(1-1-2) Collector The collector 6 is disposed on the downstream side of the apparatus main body 2. The collector 6 constitutes a second inner cylinder 61 as a second cylinder constituting the downstream side of the inner cylinder 21 and a downstream side of the outer cylinder 22, and is disposed outside the second inner cylinder 61. The second outer cylinder 62 arranged, the temperature adjusting heater 63 arranged outside the second outer cylinder 62, and the third as a collection area expanding member arranged inside the second inner cylinder 61 A cylindrical body 70.

FIG. 3 shows a cross-sectional view of the second inner cylinder 61 and the second outer cylinder 62 of the collector 6. 4 shows a cross-sectional view of the second inner cylindrical body 61 and the second outer cylindrical body 62 of the collector 6 on the downstream side of the position of the cross section of FIG.
The second inner cylinder 61, the third cylinder 70, and the second outer cylinder 62 are formed in a cylindrical shape. In the present embodiment, the second outer cylinder 62 is formed in an integral cylindrical shape with the first outer cylinder 52.

In the present embodiment, the second inner cylinder 61 includes three cylindrical collection cylinders, specifically, the first collection cylinder 61A, the second collection cylinder 61B, and the first collection cylinder in order from the upstream side. The three collecting cylinders 61C are configured to be divided and connected. The first collection cylinder 61A and the third collection cylinder 61C have the same structure.
The inside of the first collection cylinder 61A is the first collection chamber R1, the inside of the second collection cylinder 61B is the second collection chamber R2, and the inside of the third collection cylinder 61C is The third collection chamber R3 is formed, and the collection chambers R1, R2, and R3 are continuously formed in the horizontal direction toward the downstream side and communicate with each other.

  The third cylinder 70 has an axial direction along the axial direction of the second inner cylinder 61, and is disposed at the center of the cross section inside the second inner cylinder 61. A flow path of the organic EL element material is formed between the outer surface of the three-cylinder body 70, and the organic material flowing through the central portion of the cross section of the second inner cylinder body 61 is easily flowed into the flow path. Moreover, since the third cylinder 70 is cylindrical, the surface thereof extends along the axial direction of the second inner cylinder 61.

FIG. 5 shows a perspective view of the collection cylinders 61A and 61C, and FIG. 6 shows a perspective view of the second collection cylinder 61B.
As described above, as the second inner cylinder 61 can be divided into three collection cylinders, the third cylinder 70 also has a collection cylinder as shown in FIGS. 5 and 6. It is divided into three small cylinders 70A, 70B and 70C together with the bodies 61A, 61B and 61C. The small cylinders 70A, 70B, and 70C are cylindrical with the same size.

As shown in FIGS. 3 to 6, a plurality of ribs 711 and 712 are provided on the outer surface of the third cylindrical body 70. The ribs 711 and 712 are formed in a plate shape extending over the axial direction of the third cylinder. Further, the surfaces of the plurality of ribs 711 and 712 extend along the axial direction of the second inner cylinder 61.
As shown in FIGS. 3 and 5, four ribs 711 are provided on the outer surfaces (upper surface, bottom surface, and side surfaces) of the small cylinders 70A and 70C, and the collecting cylinders 61A and 61C are formed from the outer surfaces. It extends in the vertical and horizontal directions toward the inner surface, and is connected to the inner surfaces of the collecting cylinders 61A and 61C.
As shown in FIGS. 4 and 6, the rib 712 extends obliquely from the outer surface of the small cylinder 70B toward the inner surface of the second collection cylinder 61B, and the inner surface of the second collection cylinder 61B. Connected to.
Here, when the second inner cylinder 61 is viewed from the upstream side toward the downstream side in a state where the collection cylinders 61A, 61B, 61C are connected, the rib 711 and the rib 712 have a protruding direction. It is provided differently. As shown in FIG. 3, the rib 712 of the small cylinder 70B indicated by a two-dot chain line extends in an oblique direction with respect to the rib 711 extending in the vertical direction and the horizontal direction of the small cylinders 70A and 70C. The protruding directions of the ribs are different between 70A and 70C and the adjacent small cylinder 70B. Similarly in FIG. 4, the ribs 711 of the small cylinders 70A and 70C indicated by the two-dot chain lines extend in the vertical direction and the horizontal direction with respect to the rib 712 extending in the oblique direction of the small cylinder 70B.

  The flow path of the organic EL element material formed between the inner surface of the second inner cylinder 61 and the outer surface of the third cylinder 70 is a plate-like rib 711, 712 extending in the axial direction of the third cylinder 70. Can be divided into a plurality of smaller channels extending in the axial direction, that is, a divided channel can be formed. The collection chambers R1, R2, and R3 are also divided into four small rooms by ribs 711 and 712, respectively. If the collection cylinders 61A, 61B, 61C are connected, the small chambers divided into four communicate with each other in the axial direction.

The opening on the upstream side of the third cylinder 70 (small cylinder 70A) is a sealed cylinder provided between the second inner cylinder 61 (first collection cylinder 61A) and the first inner cylinder 51. The body 65 is sealed.
FIG. 7 shows a perspective view of the sealing cylinder 65. The sealing cylinder 65 has substantially the same shape as the first collection cylinder 61A, but is formed with a short axial length. In addition, a sealing small cylinder 75 that is formed in a cylindrical shape and has one opening at the end in the axial direction sealed by a sealing plate 751 is disposed at the center of the cross section of the sealing cylinder 65. . The axial length of the sealing small cylinder 75 is the same as that of the sealing cylinder 65. Like the rib 711, a rib 752 extending in the vertical direction and the left-right direction and connected to the sealing cylinder 65 is provided from the outer surface of the sealing cylinder 75.
When the sealing cylinder 65 is attached to the first collecting cylinder 61A, the small cylinder 70A and the sealing small cylinder 75 overlap, and the opening on the upstream side of the small cylinder 70A is formed by the sealing plate 751. Sealed.
As shown in FIG. 1, the opening on the downstream side of the third cylinder 70 (small cylinder 70C) is a seal attached to the downstream end of the second inner cylinder 61 (third collection cylinder 61C). The sealing member 76 is sealed.

  The temperature adjustment heater 63 is configured by an infrared heater or the like, and is arranged in an annular shape outside the second outer cylindrical body 62. The temperature adjustment heater 63 includes a first temperature adjustment heater 63A that adjusts the temperature of the first collection chamber R1, a second temperature adjustment heater 63B that adjusts the temperature of the second collection chamber R2, and a third collection chamber R3. A third temperature adjusting heater 63C for adjusting the temperature of the first temperature adjusting heater 63C. These temperature adjustment heaters 63A, 63B, and 63C can independently adjust the temperatures inside the collection chambers R1, R2, and R3 by a control unit 44 as a temperature adjustment heater control unit, which will be described later.

  The materials of the second inner cylinder 61, the second outer cylinder 62, the third cylinder 70, the sealing cylinder 65, the sealing small cylinder 75, the ribs 711, 712, 752 and the sealing member 76 are organic. It is preferable to be made of a material that is inert to the EL element material. In the present embodiment, the second outer cylinder 62 is made of quartz glass, and the second inner cylinder 61, the third cylinder 70, the sealing cylinder 65, the sealing small cylinder 75, and the ribs 711, 712. 752 and the sealing member 76 are made of stainless steel.

(1-1-3) Temperature Controller The temperature controller 4 includes a temperature sensor 41 that measures the temperature inside the vaporizer 5, a control unit 42 that controls the heater 53 based on the temperature information measured by the temperature sensor 41, and The temperature sensor 43 which measures the temperature inside the collector 6 and the control part 44 which controls the temperature adjustment heater 63 based on the temperature information measured with the temperature sensor 43 are provided.
The temperature sensor 41 includes a thermocouple 412 for the first cylinder inserted into the first inner cylinder 51 from the upstream end of the inner cylinder 21. The thermocouple 412 is connected to the control unit 42 disposed outside the apparatus main body 2. The temperature information measured by the thermocouple 412 is sent to the control unit 42.
The control unit 42 is connected to the heater 53 and controls heating by the heater 53 based on the temperature information input from the temperature sensor 41.

The temperature sensor 43 includes three thermocouples 432A, 432B, and 432C for the second cylinder inserted into the second inner cylinder 61 from the downstream end of the inner cylinder 21. The thermocouples 432A, 432B, and 432C are connected to the control unit 44 disposed outside the apparatus main body 2. The temperature information measured by the thermocouples 432A, 432B, and 432C of the temperature sensor 43 is sent to the control unit 44.
The thermocouple 432A is arranged inside the first collection chamber R1, the thermocouple 432B is arranged inside the second collection chamber R2, and the thermocouple 432C is arranged inside the third collection chamber R3. ing.

  The control unit 44 is connected to the temperature adjustment heater 63 and controls heating by the temperature adjustment heater 63 based on the temperature information input from the temperature sensor 43. In the present embodiment, the control unit 44 independently controls the temperature adjustment heaters 63A, 63B, and 63C for the collection chambers R1, R2, and R3. For example, the control unit 44 controls the temperature adjustment heaters 63A, 63B, and 63C so that the temperature varies continuously or stepwise from the first collection chamber R1 side to the third collection chamber R3 side.

(1-2) Organic EL element material The organic EL element material to be purified is a material used for the organic EL element and is not particularly limited.

(2) Purification method using a purification device A method for purifying an organic EL element material using the purification device 1 will be described.
First, a solid powder sublimable organic EL element material is accommodated in the accommodating portion 54.
Next, the cover parts 23 and 24 are attached and the inside of the vaporizer | carburetor 5 and the collector 6 is sealed.
Next, the temperature sensor 41 (thermocouple 412) is inserted into the first inner cylinder 51 from the upstream end of the vaporizer 5. On the other hand, the temperature sensor 43 (thermocouples 432A, 432B, 432C) is inserted into the second inner cylinder 61 from the downstream end of the collector 6.
Next, the inside of the apparatus main body 2 is decompressed to 10 ⁻¹ Pa or less by the vacuum pump 3.
After depressurization, the first inner cylinder 51 is heated by the heater 53, and the second inner cylinder 61 is heated by the temperature adjustment heater 63 to adjust the temperature. At this time, the temperature controller 4 controls heating by the heater 53 and the temperature adjusting heater 63 based on the temperature information measured by the temperature sensor 41 and the temperature sensor 43. Specifically, the heater 53 heats the first inner cylinder 51 to a temperature (sublimation temperature) at which the solid powder organic EL element material sublimates (changes from solid to gas) and maintains the temperature. . The temperature adjustment heaters 63A, 63B, and 63C are heated to a predetermined temperature independently of each other to adjust the temperatures of the first collection chamber R1, the second collection chamber R2, and the third collection chamber R3. In the present embodiment, the temperature of the first collection chamber R1 is adjusted slightly higher than the temperature at which the organic EL element material to be purified changes from gas to solid, and the second collection chamber R2 is lower than the same temperature. The temperature is adjusted, and the temperature of the third collection chamber R3 is adjusted to be lower than that of the second collection chamber R2.

The solid-powder organic EL element material accommodated in the accommodating portion 54 is vaporized when the accommodating portion 54 is heated and held to the sublimation temperature. The gaseous organic EL element material moves to the collector 6 side, and is solidified and collected on the inner surface of the second inner cylinder 61 corresponding to each of the collection chambers R1, R2, and R3.
In this embodiment, each collection chamber R1, R2, R3 is heated and held in the above-described relationship with respect to the vaporization (sublimation) 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 R2 heated and held at a temperature lower than the vaporization (sublimation) temperature. In the first collection chamber R1 and the third collection chamber R3, the impurity components contained in the organic EL element material supplied to the storage portion 54 are concentrated and collected.

(3) Effects of the Embodiment According to the purification device 1 and the purification method using the purification device 1 according to the first embodiment, the following effects can be obtained.

According to the refining device 1, the third cylinder 70 as the collection area expanding member is disposed inside the second inner cylinder 61. A vacuum pump 3 is connected to the downstream end of the collector 6. Therefore, an air flow is generated from the inside of the first inner cylinder 51 to the inside of the second inner cylinder 61 by the vacuum pump 3, and the gaseous organic EL element material is formed on the inner surface of the second inner cylinder 61 and the third inner cylinder 61. It contacts the surface of the cylindrical body 70 and is solidified and collected. In addition, the organic EL element material is formed between the inner surface of the second inner cylinder 61 and the outer surface of the third cylinder 70, and flows through a flow path extending in the axial direction of the second inner cylinder 61. The exhaust resistance is small, and the organic EL element material can be efficiently distributed downstream in a short time.
Therefore, according to the refiner 1, the organic EL element material can be collected not only on the inner surface of the second inner cylinder 61 but also on the surface of the third cylinder, and the purification efficiency can be improved.

  According to the refining device 1, the third cylinder 70 is disposed at the center of the cross section of the second inner cylinder 61. Therefore, the organic EL element material to be distributed through the central portion of the cross section contacts the third cylindrical body 70 or flows closer to the inner surface of the second inner cylindrical body 61 while avoiding the third cylindrical body 70. It becomes like this. As a result, the organic EL element material easily comes into contact with the inner surface of the second cylinder or the surface of the third cylinder. Therefore, according to the present invention, the purification efficiency of the organic EL element material can be improved.

According to the refining device 1, the upstream opening of the third cylinder 70 (small cylinder 70A) is sealed by the sealing plate 751 of the sealing cylinder 65, and the third cylinder 70 (small cylinder 70C). ) On the downstream side is sealed by a sealing member 76. Therefore, the space inside the second inner cylinder 61 through which the organic EL element material can be distributed can be reduced. And the airflow which goes to the inside of the 2nd inner cylinder 61 from the inside of the 1st inner cylinder 51 does not pass the inside of the 3rd cylinder 70, but the inner surface of the 2nd inner cylinder 61, the outer surface of the 3rd cylinder 70, and Pass between.
Therefore, according to the refining device 1, the organic EL element material can be efficiently collected on the inner surface of the second inner cylinder 61 and the outer surface of the third cylinder 61, and the purification efficiency can be further improved.
Moreover, according to the refiner | purifier 1, since the organic EL element material is selectively collected by the inner surface of the 2nd inner cylinder 61, and the outer surface of the 3rd cylinder 70, the collection | recovery operation | work after refinement | purification is easy. Become.

  According to the purification apparatus 1, an organic EL formed between the inner surface of the second inner cylinder 61 and the outer surface of the third cylinder 70 by the plurality of ribs 711 and 712 provided on the outer surface of the third cylinder. The flow path of the element material can be a plurality of divided flow paths extending in the axial direction. As a result, the organic EL element material is collected on the inner surface of the second inner cylindrical body 61, the outer surface of the third cylindrical body 70, and the surfaces of the ribs 711 and 712 while passing through the divided flow path. Become. Therefore, according to the purification apparatus 1, the purification efficiency of the organic EL element material can be further improved.

  According to the refining device 1, the plurality of ribs 711 and 712 protrude from the outer surface of the third cylinder 70 toward the inner surface of the second inner cylinder 61 from the upstream side to the downstream side of the third cylinder 70. Since it is provided so as to be different on the way to, the divided flow path can be formed in a meandering shape. As a result, since the organic material flows toward the downstream side while meandering through the divided flow path, the organic material is further collected on the inner surface of the second inner cylinder 61, the outer surface of the third cylinder 70, and the surfaces of the ribs 711 and 712. It becomes easy to be done. Therefore, according to the purification apparatus 1, the purification efficiency of the organic material can be further improved.

<Second embodiment>
Next, the refiner | purifier of the organic EL element material which concerns on 2nd embodiment of this invention is demonstrated. In the following description, the same parts as those already described are denoted by the same reference numerals, and the description thereof is omitted or simplified.

FIG. 8 shows a perspective view of the second inner cylinder 67 provided in the organic material refining device according to the second embodiment, and FIG. 9 shows a third cylinder arranged inside the second inner cylinder 67. A perspective view of the body 72 is shown.
The second inner cylinder 67 is substantially the same in shape as the second inner cylinder 61 of the first embodiment, but the second inner cylinder 67 is different in that it can be divided into two parts. .
The third cylinder 72 as the collection area expanding member has substantially the same shape as the third cylinder 70 of the first embodiment, but the third cylinder 72 is formed so as to be divided into two. It is different in point.
The other points are almost the same as those of the purification apparatus 1 of the first embodiment, and thus the description is omitted or simplified.

As shown in FIG. 8, the cylindrical second inner cylindrical body 67 includes a semicircular body 671 and a semicircular body 672 that are divided into two along the axial direction and are connected by a connecting tool 673 such as a hinge. Yes. When the two semicircular bodies 671 and 672 are combined into a cylindrical shape, the connector 673 is positioned on the outer surface of the second inner cylindrical body 67.
As shown in FIG. 9, the cylindrical third cylindrical body 72 is similarly connected to a semicircular body 721 and a semicircular body 722 that are divided into two along the axial direction by a connecting tool 723 such as a hinge. Has been. When the two semicircular bodies 721 and 722 are combined into a cylindrical shape, the connector 723 is positioned on the inner surface of the third cylindrical body 72. The rib 711 is detachably attached to the semicircular bodies 721 and 722 by screws or the like .

  When refining the organic EL element material, the two semicircular bodies 671, 672 are combined to form the second inner cylindrical body 67, the two semicircular bodies 721, 722 are combined to form the third cylindrical body 72, and the second The third cylinder 72 is inserted into the inner cylinder 67 and the end of the rib 711 is fixed to the inner surface of the second inner cylinder 67 with a screw (not shown).

According to the organic EL element material refining device according to the second embodiment, in addition to the same effects as those of the first embodiment, the following effects can be obtained.
According to the organic EL element material refining device according to the second embodiment, the second inner cylindrical body 67 and the third cylindrical body 72 are formed so as to be split into two so that they can be divided into each. . Therefore, it becomes easier to collect the organic EL element material as compared with the case where the collection surface remains a cylindrical body.
Further, since the rib 711 is detachably attached to the semicircular bodies 721 and 722 by screws or the like, the recovery of the organic EL element material is further facilitated.

<Third embodiment>
Next, an organic EL element material purification apparatus 1A according to a third embodiment of the present invention will be described. In the following description, the same parts as those already described are denoted by the same reference numerals, and the description thereof is omitted or simplified.

  FIG. 10 is a schematic cross-sectional view of an organic material purification apparatus according to the third embodiment. The refiner | purifier 1A of the organic EL element material which concerns on 3rd embodiment differs in the shape of the collection area expansion member arrange | positioned inside the 2nd inner cylinder 61 from the said embodiment. Since the other points are almost the same, the description is omitted or simplified.

The collection area expanding member used in the purification apparatus 1A is a lattice member 80 in which a plurality of plate-like members 81 extending in the axial direction of the second inner cylinder 61 are combined in a lattice shape.
FIG. 11 is a schematic cross-sectional view of the collector 6 of the purification apparatus according to the third embodiment.
As shown in FIG. 11, the lattice member 80 includes a plurality of plate-like members 81 arranged in a substantially horizontal direction and a plurality of plate-like members 81 arranged in a substantially vertical direction combined in a lattice shape. Is formed. The end of each plate-like member 81 is in contact with the inner surface of the second inner cylinder 61.
Also by the lattice member 80, the flow path of the organic EL element material inside the second inner cylinder 61 can be a plurality of divided flow paths extending in the axial direction. The collection chambers R1, R2, and R3 are also divided into a large number of small chambers (honeycomb shapes) by the lattice member 80.
As described above, since the second inner cylinder 61 can be divided into three collection cylinders, the grid member 80 is also divided into three grid members together with the collection cylinders 61A, 61B, 61C. It is made possible. In the present embodiment, the vaporized organic EL element that circulates in the central portion of the cross section of the second inner cylinder 61 without attaching the sealing cylinder 65 as in the first embodiment to the upstream side of the lattice member 80. The material is introduced into a number of small chambers of the lattice member 80.

According to the organic EL element material refining device 1A according to the third embodiment, the following effects can be obtained.
According to the purification apparatus 1 </ b> A, the lattice member 80 as a collection area expanding member is disposed inside the second inner cylindrical body 61. Therefore, the flow path of the organic EL element material inside the second inner cylindrical body 61 can be a plurality of divided flow paths extending in the axial direction. As a result, the organic EL element material flows through the flow path between the inner surface of the second inner cylinder 61 and the outer surface of the lattice member 80 or the flow path surrounded by the plate-like members 81 of the lattice member 80, It is efficiently collected on the inner surface of the inner cylinder 61 and the surface of the plate-like member 81. Moreover, since the said flow path extended toward the axial direction of the 2nd inner cylinder 61 passes, the organic EL element material can be distribute | circulated efficiently downstream in a short time.
Therefore, according to the refining device 1, the organic EL element material can be collected not only on the inner surface of the second inner cylinder 61 but also on the surface of the lattice member 80, and the refining efficiency can be improved.

  Further, according to the refining device 1A, the lattice member 80 is configured by combining the plate-like members 81. Therefore, after refining the organic EL element material, the lattice member 80 is disassembled into a plurality of plate-like members 81. If it is recovered from the above, the efficiency of the recovery work can be improved.

<Modification of Embodiment>
In addition, this invention is not limited to embodiment mentioned above, In the range which can achieve the objective of this invention, the deformation | transformation etc. which are shown below are included.

As a collection area expansion member, it is not limited to the aspect demonstrated by the said embodiment.
For example, the configuration of the lattice member 80 as described in the third embodiment may be changed as follows. FIG. 12 is a perspective view illustrating the shape of a lattice member 80A as a collection area expanding member according to a modification of the embodiment.
As shown in FIG. 12, the lattice member 80A includes a region S1 composed of a plurality of vertical plate members 82 arranged in a substantially vertical direction and a plurality of horizontal plate members 83 arranged in a substantially horizontal direction. It is good also as the shape which provided alternately area | region S2 in the axial direction of the 2nd inner cylinder 61. As shown in FIG. When such a lattice member 80A is arranged inside the second inner cylinder 61 and viewed from the upstream side to the downstream side of the second inner cylinder 61, as shown in the cross-sectional view of FIG. A vertical plate member 82 and a horizontal plate member 83 are arranged on the upper side.
When the lattice member 80A is disposed inside the second inner cylinder 61, the organic EL element material flows between the second inner cylinder 61 and the vertical plate member 82 or between the vertical plate members 82, It passes through the area S1, and then flows into the area S2. In the region S2, the organic EL element material flows between the second inner cylinder 61 and the horizontal plate member 83 or between the horizontal plate members 83, passes through the region S2, and is then provided. Flow into the area S1. Therefore, the organic EL element material meanders when it flows from the region S1 to the region S2. As a result, the organic EL element material can be more easily brought into contact with the inner surface of the second inner cylinder 61 and the surface of the lattice member 80A. Therefore, the purification efficiency can be improved by arranging the lattice member 80A. Moreover, it is preferable that the lattice member 80A is also assembled so as to be divided by the vertical plate member 82 and the horizontal plate member 83, and is decomposed after purification to recover the organic EL element material.

The third cylinder as the collection area expanding member is not limited to the cylindrical body as described in the above embodiment. In addition, it can be a shape such as a cylindrical body having an elliptical cross section, a polygonal cross section (triangle, quadrangle, pentagon, octagon, etc.).
Moreover, as a collection area expansion member, as shown in FIG. 14, the shape which crossed the plate-shaped member 90 extended along the axial direction of the 2nd inner cylinder 61 may be sufficient. FIG. 14 shows a plate-like member 90 in which a vertical plate member 91 arranged in the vertical direction inside the second inner cylinder 61 and a horizontal plate member 92 arranged in the horizontal direction intersect in a cross shape. Has been. Also with such a plate-like member 79, the flow path of the organic EL element material can be made into four divided flow paths, so that the purification efficiency can be improved as described above.

  In the above-described embodiment, the inner cylindrical body 21 and the outer cylindrical body 22 have been described by taking a cylindrical shape as an example. However, for example, any shape such as a box shape, a cylindrical shape, a tank shape, a cubic shape, and the like can be given. . In addition, examples of the cross-sectional shapes of the inner cylinder body 21 and the outer cylinder body 22 include shapes such as a circle, a quadrangle, and a semicircle. Moreover, the cross-sectional shape may be constant or the cross-sectional shape may be partially different. Further, the inner cylinder 21 and the outer cylinder 22 do not have to have the same cross-sectional shape.

Moreover, in the said embodiment, although the example which comprises the 2nd inner cylinder 61 by three collection cylinders was mentioned as an example, it was not limited to such an aspect. For example, an integrally formed second inner cylinder may be used.
In the above embodiment, the structure in which the apparatus main body 2 houses the inner cylindrical body 21 inside the outer cylindrical body 22 has been described as an example. However, the present invention is not limited to such a mode. It is good also as an aspect which has arrange | positioned the collection area expansion member inside the inner cylinder 21 without providing.

  In the second embodiment, the second inner cylindrical body 67 and the third cylindrical body 72 are formed so as to be split into two, but are not limited thereto, and may be formed so as to be further finely divided.

In the above-described embodiment, quartz glass is mainly described as an inactive material with respect to the organic EL element material. However, the present invention is not limited to this. For example, stainless steel, tantalum, tungsten, molybdenum, titanium, or the like can be used as the inert metal, and quartz, zirconia, alumina, boron nitride, silicon nitride, or the like can be used as the ceramic. In addition, carbon, Teflon (registered trademark), or the like can be used.
Further, 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 | part which an organic EL element material contacts, and it may also comprise with another material about the other site | part.

  The heating means and heating method for heating the vaporizer 5 and the collector 6 are not limited to those described in the above embodiment. As 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. For example, when heating by the induction heating method, the vaporizer and the collector are made of a material that generates heat by electromagnetic induction, such as stainless steel.

  In the said embodiment, although the 2nd inner cylinder 61 of the collector 6 demonstrated and demonstrated the example divided into three collection chamber R1, R2, R3, it 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.

  The setting of the heating temperature for each of the collection chambers R1, R2, and R3 of the collector 6 is not limited to that described in the above embodiment.

In the above-described embodiment, the powdery organic EL element material is accommodated in the accommodating portion 54 and is purified by vaporization. However, the liquid material is accommodated in the accommodating portion 54 and is purified by vaporization. Also good.
The organic material purified by the purification apparatus of the present invention is not limited to the organic EL element material. In addition, the organic material purified by the purification apparatus of the present invention may be repeatedly purified to further increase the purity.

  The present invention can be used for refining organic materials such as materials for organic EL devices.

1 ... Organic material purification equipment 3 ... Vacuum pump (exhaust device)
5 ... Vaporizer 51 ... First inner cylinder (first cylinder)
53 ... Heater 6 ... Collector 61 ... Second inner cylinder (second cylinder)
63 ... Temperature adjusting heater 70 ... Third cylinder (collecting area expanding member)
711, 712 ... rib 80 ... lattice member (collecting area expanding member)
R1, R2, R3 ... Collection room

Claims (11)

A vaporizer including a first cylinder to which an organic material is supplied, and a heater disposed on the outside of the first cylinder to vaporize the supplied organic material;
A second cylinder communicating with the first cylinder of the vaporizer; and a temperature adjusting heater disposed outside the second cylinder for adjusting the temperature of the second cylinder; vaporizing by the vaporizer A collector for collecting the gaseous organic material on the inner surface of the second cylinder;
A collection area expanding member disposed inside the second cylinder, having a surface extending along the axial direction of the second cylinder, and increasing a contact area with the gaseous organic material;
An exhaust device connected to the downstream end of the collector , and
The collection area expanding member is a cylindrical third cylinder,
The axial direction of the third cylinder is along the axial direction of the second cylinder,
A plurality of ribs extending over the axial direction of the third cylinder are provided on the outer surface of the third cylinder,
The plurality of ribs are provided such that a direction protruding from the outer surface of the third cylinder toward the inner surface of the second cylinder is different on the way from the upstream side to the downstream side of the third cylinder. purification device of an organic material characterized in that there.   A vaporizer including a first cylinder to which an organic material is supplied, and a heater disposed on the outside of the first cylinder to vaporize the supplied organic material;
  A second cylinder communicating with the first cylinder of the vaporizer; and a temperature adjusting heater disposed outside the second cylinder for adjusting the temperature of the second cylinder; vaporizing by the vaporizer A collector for collecting the gaseous organic material on the inner surface of the second cylinder;
  A collection area expanding member disposed inside the second cylinder, having a surface extending along the axial direction of the second cylinder, and increasing a contact area with the gaseous organic material;
  An exhaust device connected to the downstream end of the collector, and
  The collection area expanding member is a cylindrical third cylinder,
  The axial direction of the third cylinder is along the axial direction of the second cylinder,
  Openings at both ends of the third cylinder are sealed
  An organic material refining device.   A vaporizer including a first cylinder to which an organic material is supplied, and a heater disposed on the outside of the first cylinder to vaporize the supplied organic material;
  A second cylinder communicating with the first cylinder of the vaporizer; and a temperature adjusting heater disposed outside the second cylinder for adjusting the temperature of the second cylinder; vaporizing by the vaporizer A collector for collecting the gaseous organic material on the inner surface of the second cylinder;
  A collection area expanding member disposed inside the second cylinder, having a surface extending along the axial direction of the second cylinder, and increasing a contact area with the gaseous organic material;
  An exhaust device connected to the downstream end of the collector;
An outer cylinder that houses the first cylinder and the second cylinder,
  The collection area expanding member is a cylindrical third cylinder,
  The axial direction of the third cylinder is along the axial direction of the second cylinder,
  The heater is disposed outside the first cylinder and the outer cylinder,
  The temperature adjusting heater is disposed outside the second cylinder and the outer cylinder.
  An organic material refining device. In the refiner | purifier of the organic material of Claim 1 or Claim 3,
The organic material refining device, wherein openings at both ends of the third cylindrical body are sealed. In the refiner | purifier of the organic material of Claim 2 or Claim 3 ,
A plurality of ribs extending in the axial direction of the third cylinder are provided on the outer surface of the third cylinder. In the refiner | purifier of the organic material of Claim 5,
The plurality of ribs are provided such that a direction protruding from the outer surface of the third cylinder toward the inner surface of the second cylinder is different on the way from the upstream side to the downstream side of the third cylinder. An organic material refining device characterized by that. In the refiner | purifier of the organic material of Claim 1 or Claim 2 ,
An outer cylinder that houses the first cylinder and the second cylinder;
The heater is disposed outside the first cylinder and the outer cylinder,
The said temperature control heater is arrange | positioned on the outer side of said 2nd cylinder and the said outer cylinder. The refiner | purifier of the organic material characterized by the above-mentioned. In the refiner | purifier of the organic material as described in any one of Claim 1- Claim 7 ,
The said collection area expansion member is arrange | positioned in the cross-sectional center part of said 2nd cylinder. The refiner | purifier of the organic material characterized by the above-mentioned. In the refiner | purifier of the organic material as described in any one of Claim 1- Claim 8 ,
The said collection area expansion member is formed so that division | segmentation is possible. The refiner | purifier of the organic material characterized by the above-mentioned. In the refiner | purifier of the organic material as described in any one of Claim 1- Claim 9 ,
The said 2nd cylinder is formed so that division | segmentation is possible. The refiner | purifier of the organic material characterized by the above-mentioned. In the refiner | purifier of the organic material as described in any one of Claim 1- Claim 10 ,
The said 2nd cylinder and the said collection area expansion member are formed with the inert metal or ceramics. The refiner | purifier of the organic material characterized by the above-mentioned.

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