WO2013065627A1

WO2013065627A1 - Apparatus for purifying organic material

Info

Publication number: WO2013065627A1
Application number: PCT/JP2012/077853
Authority: WO
Inventors: 雅温伊藤; 泰憲門井; 芳賀　亮
Original assignee: 出光興産株式会社
Priority date: 2011-10-31
Filing date: 2012-10-29
Publication date: 2013-05-10
Also published as: KR101943140B1; TW201323045A; JP2013116464A; KR20140084166A; JP5886674B2

Abstract

This apparatus for purifying an organic material is characterized by being provided with: an evaporator (5) that is provided with a first inner cylindrical body (51), into which an organic EL element material is supplied, and a heating heater (53) that is arranged outside the first inner cylindrical body (51) and evaporates the supplied organic EL element material; a collector (6) that is provided with a second inner cylindrical body (61) that communicates with the first inner cylindrical body (51) of the evaporator (5) and a temperature-regulating heater (63) that is arranged outside the second inner cylindrical body (61) and regulates the temperature of the second inner cylindrical body (61), said collector (6) collecting the organic material, which has been evaporated by the evaporator (5) and in a gaseous state, on the inner surface of the second inner cylindrical body (61); a vacuum pump (3) that is connected to the downstream of the collector (6); and shielding members (25) that are arranged at the both ends of an inner cylindrical body (21), which is configured of the first inner cylindrical body (51) and the second inner cylindrical body (61) communicating each other, and have open portions and closed portions.

Description

Organic material purification equipment

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 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. Therefore, in order to reduce impurities, it is necessary to purify the organic EL element material with high purity.

For example, Patent Document 1 discloses a purification apparatus for purifying an organic EL element material. 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, while arrange | positioning the cell by which the refinement | purification target substance was hold | maintained in the 1st area, pressure-reducing inside the apparatus, flowing carrier gas, and heating the 1st area. Sublimate the substance to be purified. Impurities from 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 partition hole holes and moves to the other sections. Purified.

In the refining device described in Patent Document 2, a plurality of rectifying plates are provided in the inner cylinder through which the sublimated organic material flows so that the openings do not overlap each other in the axial direction. 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 JP2011-508553A

However, the partition walls of Patent Document 1 and the rectifying plate of Patent Document 2 are both provided in a cylinder through which the sublimated organic material circulates to partition the inside of the cylinder, and the organic material can be recovered for each component in the partitioned section. It is provided as follows. Therefore, the organic material that has not been collected in each section is discharged from the most downstream section to the outside of the refining apparatus, resulting in a problem that the yield is reduced. Moreover, in the refinement | purification apparatus described in patent document 1 and patent document 2, control of the temperature of each area is only performed by heating with a heater etc., and fully prevents the temperature fall of a collection cylinder edge part. There was a problem that the yield and purity of the organic material were lowered.

The purpose of the present invention is to prevent the organic material to be purified from being discharged to the outside of the purifier and to prevent the temperature at the end inside the purifier from decreasing, thereby improving the yield and purity of the purified organic material. An object of the present invention is to provide an organic material purification apparatus that can be improved.

The organic material refining device of the present invention is a vaporizer equipped with a first cylinder to which an organic material is supplied, and a heater that is disposed outside the first cylinder and vaporizes the supplied organic material. And a second cylinder communicating with the first cylinder of the vaporizer, and a temperature adjusting heater arranged outside the second cylinder for adjusting the temperature of the second cylinder, the vaporizer A collector that collects the gaseous organic material vaporized at the inner wall of the second cylinder, an exhaust device connected to a downstream side of the collector, the first cylinder, and the second cylinder It is provided with the shielding member which is installed in the both ends of the inner cylinder formed in communication with a cylinder, and has an opening part and a closure part.

According to the present invention, the first cylinder is provided by providing the shielding member having the opening and the closing part at both ends of the inner cylinder formed by communicating the first cylinder and the second cylinder. The organic material, which is the object of purification, can be prevented from flowing out of the inner cylinder while keeping the body and the second cylinder at a high vacuum, and the organic material collected on the inner wall of the second cylinder can be collected. The rate can be improved.
Here, the yield of the organic material refers to the recovery rate of the organic material that satisfies a certain purity that can be used as a product.

In the organic material refining device of the present invention, it is preferable that an outer cylinder that houses the inner cylinder is provided, and the shielding member is further provided at both ends of the outer cylinder.

ADVANTAGE OF THE INVENTION According to this invention, the yield and purity of the organic material collected with the inner wall of a 2nd cylinder can be improved more, suppressing the temperature fall of the both ends inside a refiner | purifier.

Further, in the organic material refining device of the present invention, it is preferable that an area ratio between the opening and the blocking portion in the shielding member is 5:95 to 50:50.

According to the present invention, it is possible to prevent the organic material from being discharged directly to the outside of the refining device without being collected by the wall of the second cylinder.

Furthermore, in the organic material refining device of the present invention, the opening of the shielding member (hereinafter referred to as a heat shielding member) of the outer cylinder forms a plurality of through holes radially from the central portion of the shielding member. Thus, an opening of the shielding member (hereinafter referred to as a material shielding member) of the inner cylindrical body forms a through hole having a shape surrounded by a circle or an arc and a straight line connecting both ends of the arc. It is preferable to become.

According to the present invention, while the high shielding of the first cylinder and the second cylinder is maintained with the material shielding member while the temperature shielding at the both ends inside the purification apparatus is suppressed by the heat shielding member, The discharge of a certain organic material to the outside of the purification apparatus can be prevented, and the yield and purity of the organic material collected on the inner wall of the second cylinder can be improved.

In the organic material refining device of the present invention, the shielding member (the heat shielding member and the material shielding member) includes a plurality of shielding plates that are spaced apart from each other, and the plurality of shielding plates are respectively It is preferable that the openings are provided, and the openings of the adjacent shielding plates do not overlap each other when the shielding plates are viewed from the orthogonal direction.

According to the present invention, when the shielding plates are viewed from the orthogonal direction, the openings of the adjacent shielding plates do not overlap. Therefore, when the airflow containing the organic material passes through the opening and proceeds straight as it is, it comes into contact with the blocking portion of the adjacent shielding plate. And the airflow containing an organic material will meander through the space | interval of the shielding board arranged at intervals, and toward the opening part of the said adjacent shielding board. In this way, since the airflow containing the organic material meanders without going straight toward the discharge device, the amount of the organic material sucked by the exhaust device from the inside of the device is suppressed, and the yield can be improved. .
The orthogonal direction of the shielding plate is a direction orthogonal to the surface of the shielding plate, that is, equal to the thickness direction.

Furthermore, in the organic material refining device of the present invention, a raw material container to which the organic material is supplied is installed inside the first cylinder, and the first cylinder is in communication with the second cylinder. Is an end on the opposite side, and the shielding member (material shielding member) installed on the upstream side of the raw material container preferably has no opening.

According to the present invention, there is provided a shielding member made of a material having no opening at an end portion of the first cylindrical body opposite to the side communicating with the second cylindrical body and upstream of the raw material container. By providing, it is possible to prevent the organic material from flowing out of the first cylindrical body, change the flow direction of the organic material toward the upstream side from the raw material container, and the organic material toward the downstream side. Can be promoted. Therefore, the yield of the organic material on the inner wall of the second cylinder can be improved.

The cross-sectional schematic of the refiner | purifier which concerns on 1st embodiment of this invention. The top view of the shielding member (shielding member of material) in said 1st embodiment. The top view of the shielding member (thermal shielding member) in said 1st embodiment. The perspective view which represented typically the shielding member (shielding member of material) in 2nd embodiment of this invention. The top view of the shielding member (shielding member of material) which concerns on the modification of this invention. The perspective view which represented typically the shielding member (shielding member of material) which concerns on the modification of this invention. The perspective view which represented typically the shielding member (shielding member of material) which concerns on the modification of this invention. The perspective view which represented typically the shielding member (shielding member of material) which concerns on the modification of this invention. The top view of the shielding member (heat shielding member) which concerns on the modification of this invention. The cross-sectional schematic diagram which represented typically the shielding member (thermal shielding member) which concerns on the modification of this invention. The top view of the shielding member (heat shielding member) which concerns on the modification of this invention. The top view of the shielding member (heat shielding member) which concerns on the modification of this invention. The perspective view which represented typically the shielding member (thermal shielding member) which concerns on the modification of this invention.

Embodiments of the present invention will be described below with reference to the drawings.
<First embodiment>
(1) Structure of refinement | purification apparatus The cross-sectional schematic 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, and a vacuum pump 3 as an exhaust device for reducing the pressure inside the device main body 2. Hereinafter, the case where the organic EL element material as the organic material is purified will be described as an example.

(1-1) Apparatus Main Body The apparatus 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 having a double tube structure in which both ends of the outer cylindrical body 22 are closed with

lid portions

23 and 24, and a shielding portion 25 is provided inside.
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. As shown in FIG. 1, a vacuum pump 3 is connected to the end of the apparatus main body 2 on the collector 6 side. 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 back portion of the apparatus main body 2. In the present 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 organic EL element material flows into the collector 6 by suction of the vacuum pump 3. It is solidified by the collector 6 and collected. 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.
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.). In the present embodiment, the apparatus main body 2 is made of quartz glass.

(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.
The first inner cylinder 51 and the first outer cylinder 52 are each formed in a cylindrical shape.
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 at the substantially central portion of the cross section inside the cylinder of the first inner cylindrical body 51. The shape of the accommodating part 54 may be any shape, for example, it is formed in a dish shape having a bottom surface of a semi-cylindrical or quadrangular plate shape, and a side surface standing in an out-of-plane direction from the periphery of the bottom surface, It contains a solid organic EL element material such as powder.
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 made of quartz glass. Is done.

(1-1-2) Collector The collector 6 is disposed downstream of the apparatus 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. A second outer cylindrical body 62 disposed and a temperature adjusting heater 63 disposed outside the second outer cylindrical body 62 are provided.
The second inner cylinder 61 and the second outer cylinder 62 are each formed in a cylindrical shape.
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 61 </ b> A is connected to the first inner cylinder 51. 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 continuously in the horizontal direction toward the downstream side, and communicates with each other. Each collection chamber R1, R2, R3 condenses the gaseous organic EL element material vaporized by the vaporizer 5, and collects it as solidified or liquefied organic EL element material.

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 can independently adjust the temperatures inside the collection chambers R1, R2, and R3.
The material of the second inner cylinder 61 and the second outer cylinder 62 is preferably made of a material that is inactive with respect to the organic EL element material, and is made of quartz glass in this embodiment.

(1-1-3) Shielding Section The shielding section 25 is an end portion of the inner cylindrical body 21, and includes an upstream shielding member 26 (material shielding member) installed in the first inner cylindrical body 51, and a second inner A downstream shielding member 27 (material shielding member) installed on the cylinder 61 and an end shielding member 28 (heat shielding member) installed on the end of the outer cylinder 22 are provided.
The shielding part 25 increases the amount of collection of the inner wall of the second inner cylinder of the organic EL element material, and suppresses a decrease in end temperature inside the inner cylinder 21 and the outer cylinder 22.

The upstream shielding member 26 is provided in the first inner cylinder 51 in the vicinity of the upstream end of the housing portion 54 and in the vicinity of the housing portion 54, vaporizes from the housing portion 54, and travels upstream. The direction of the air flow of the material is changed, and the organic EL element material is promoted to go downstream.
The upstream shielding member 26 includes a disk-shaped upstream shielding plate 261 having a diameter that is substantially the same as the inner diameter of the first inner cylinder 51. Thereby, when the upstream shielding member 26 is installed, the gap between the side surface of the upstream shielding plate 261 and the side surface of the first inner cylinder 51 can be reduced. The upstream shielding member 26 may be provided with an opening so that the area ratio between the opening and the blocking portion is 5:95 to 50:50, or may not be provided at all. In particular, it is preferable that no opening is provided. When no opening is provided, the organic EL element material can be further prevented from flowing out of the first inner cylinder 51, and the yield of the organic EL element material on the inner wall of the second inner cylinder 61 can be prevented. Can be improved.

The downstream shielding member 27 is installed at the end of the second inner cylinder 61 opposite to the side communicating with the first inner cylinder 51, and the organic EL element material from the second inner cylinder 61 Control spillage.
FIG. 2 shows a plan view of the downstream shielding member 27. The downstream shielding member 27 includes a disk-shaped downstream shielding plate 271 </ b> D whose diameter is substantially the same as the inner diameter of the second inner cylinder 61. A circular through hole 272D as an opening is formed in the downstream shielding plate 271D. The through hole 272D is a circle having a center at the center of the downstream shielding plate 271D.

In addition, in the downstream shielding member 27, as above-mentioned, through-hole 272D is an opening part, and parts other than through-hole 272D become a obstruction | occlusion part. If the downstream shielding member 27 is provided in this way, the flow of the material can be restricted by the closing portion to suppress the outflow of the material for the organic EL element from the inside of the second inner cylindrical body 61, and the second portion can be passed through the opening. While maintaining the degree of vacuum inside the inner cylinder 61, an air flow containing light impurities of the organic EL element material can be sucked.

In the downstream shielding member 27, the area of the opening, that is, the ratio of the area of the through hole 272D to the area of the blocking part is preferably 5:95 to 50:50. Among these, 30:70 to 50:50 is particularly preferable. By forming the opening in this manner, it is possible to suppress the organic EL element material from being directly collected to the outside of the purifier 1 without being collected on the inner wall of the second inner cylindrical body 61, and more effectively While maintaining the degree of vacuum inside the inner cylinder 61, light impurities of the organic EL element material can be sucked and exhausted downstream.

The end shielding member 28 is installed at the inner end of the outer cylinder 22 from the

lid parts

23 and 24 and shields the heat inside the outer cylinder 22, thereby lowering the temperature of the end inside the outer cylinder 22. Is suppressed, the organic EL element material of the purification object is prevented from being discharged to the outside, and the yield and purity of the organic EL element material collected on the inner wall of the second cylinder are further improved. be able to.
FIG. 3 shows a plan view of the end shielding member 28. The end shielding member 28 includes a disk-shaped end shielding plate 281 having a diameter that is substantially the same as the inner diameter of the outer cylindrical body 22. A plurality of through holes 282 as openings are formed in the end shielding plate 281. A plurality of through holes 282 are formed radially from the central portion of the end shielding plate.
In the end shielding member 28, the through hole 282 is an opening, and a portion other than the through hole 282 is a closed portion. In the end shielding member 28, the area ratio of the opening, that is, the total area of the plurality of through holes 282 and the area of the blocking part is 5:95 to 50:50.

Thus, by providing the end shielding member 28 on the inner side of the outer cylindrical body 22, it is possible to suppress the temperature drop at the end of the outer cylindrical body 22, and thus the temperature decrease of the inner cylindrical body 21 can be suppressed. Therefore, each collection chamber R1, R2, R3 can be kept at a predetermined temperature.

The materials of the upstream shielding member 26, the downstream shielding member 27, and the end shielding member 28 are preferably composed of materials that are inert to the organic EL element material. In the first embodiment, the end shielding member 28 is made of stainless steel, and the upstream shielding member 26 and the downstream shielding member 27 are made of quartz.

In the present embodiment, by providing the shielding portion 25 as described above, a decrease in the internal temperature of the outer cylindrical body 22 and the inner cylindrical body 21 is suppressed. In particular, it is possible to collect the target organic EL element material from the raw material by suppressing the temperature drop of the collection chambers R1, R2, and R3 and keeping the collection chambers R1, R2, and R3 at a predetermined temperature. it can. That is, the yield and purity of the organic EL element material collected in each of the collection chambers R1, R2, and R3 can be kept high. Here, in the present invention, the yield of the organic EL element material refers to the recovery rate of the organic EL element material that satisfies a certain purity or more. As described above, in the present embodiment, since the organic EL element material with high purity can be collected in each of the collection chambers R1, R2, and R3, the yield of the organic EL element material is improved. Can do. On the other hand, when the temperature of the collection chambers R1, R2, and R3 is significantly different from the predetermined temperature, the organic EL element material with low purity may be collected and the yield may be reduced.

(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. Among others, 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). It is done.

(2) Purification method using purification apparatus Next, a method for purifying the organic EL element material using the purification apparatus 1 will be described.
First, the powdery 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 5 and the collector 6 is sealed.
Next, the inside of the apparatus main body 2 is decompressed to 10 ⁻¹ Pa or less by the vacuum pump 3.
After decompression, 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. Specifically, the heater 53 heats the first inner cylinder 51 to a temperature at which the powdered organic EL element material is vaporized (vaporization temperature), and maintains the temperature at the temperature. The temperature adjusting heater 63 independently heats the first collection chamber R1, the second collection chamber R2, and the third collection chamber R3 to a predetermined temperature. In the present embodiment, the first collection chamber R1 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 R2 is heated to the same temperature. The third collection chamber R3 is heated and held slightly lower than the second collection chamber R2.

The liquid organic EL element material accommodated in the accommodating portion 54 is vaporized when the accommodating portion 54 is heated and held to the vaporization temperature. The gaseous organic EL element material moves to the collector 6 side and is collected by being solidified or liquefied 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 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 R2 heated and held at the same temperature as the condensation temperature. In the first collection chamber R1 and the third collection chamber R3, the impurity component contained in the raw material may be collected together with the organic EL element material.

(3) Effects of First 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.
[1] In the purification apparatus 1, since the downstream shielding member 27 having the through hole 272D is provided at the end of the second inner cylinder 61 opposite to the side communicating with the first inner cylinder 51, the second inner cylinder 61 The yield of the organic EL element material collected by the inner wall of the cylinder 61 can be improved.

[2] The ratio of the area of the through hole 272D in the downstream shielding member 27 to the area of the portion other than the through hole 272D was set to 5:95 to 50:50. Further, the through hole 272D is provided in a circular shape at the center of the downstream shielding plate 271D. Accordingly, the organic EL element material is not collected on the inner wall of the second inner cylinder 61 and is directly discharged to the outside of the refining device 1 while maintaining the degree of vacuum of the inner cylinder 21, and the organic EL Light impurities in the element material can be exhausted.

[3] Since the upstream shielding member 26 is provided on the upstream side of the housing portion 54, the organic EL element material can be prevented from flowing out of the inner cylindrical body 21 from the inside of the first inner cylindrical body 51. The organic EL element material can be prevented from going upstream from the housing portion 54, and the organic EL element material can be promoted to go downstream. Therefore, the yield of the organic EL element material can be improved.

[4] Furthermore, since the upstream shielding member 26 is not provided with an opening, it is possible to further prevent the organic EL element material from flowing out of the first inner cylinder 51. The yield at the inner wall of the second inner cylinder 61 can be further improved.

[5] Since the end shielding member 28 is installed at the inner ends of the outer cylindrical body 22 from the

lid portions

23 and 24, the temperature drop inside the outer cylindrical body 22, and hence the inner cylindrical body 21 is suppressed. be able to.

<Second embodiment>
Next, the refinement | purification apparatus 1 of the organic EL element material which concerns on 2nd embodiment of this invention is demonstrated using drawing. The second embodiment is different from the first embodiment in that a downstream shielding member 30 </ b> A is provided instead of the downstream shielding member 27. 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. 4 is a perspective view schematically showing the downstream shielding member 30A. As shown in FIG. 4, the downstream shielding member 30A includes three

downstream shielding plates

301A, 301B, and 301C. In the downstream shielding member 30A, a downstream shielding plate 271D having a through hole 274D at the center is used as the

downstream shielding plates

301A and 301C, and the downstream shielding plate 301B is formed in a disk shape without a through hole, and has a diameter larger than that of the downstream shielding plate 271D. A small downstream shielding plate 271E is used. Then, the

downstream shielding plates

271D, 271E, and 271D are arranged in this order. In this case, as indicated by an arrow in FIG. 4, the airflow flowing through the downstream shielding member 30A hits the downstream shielding plate 271E, meanders so as to bypass the downstream shielding plate 271E, and passes through. In the downstream shielding member 30A, the through hole 274D is an opening, and the portion other than the through hole 274D of the downstream shielding plate 271D and the downstream shielding plate 271E are blocking portions.
Thus, if the air flow containing the organic EL element material passes through the downstream shielding member 30A while meandering, the amount of the organic EL element material passing through the downstream shielding member 30A is limited. The Therefore, since the probability that the organic EL element material comes into contact with the inner wall of the inner cylinder 21 is increased, the yield can be improved.
In addition, by configuring the downstream shielding member 30A with the plurality of

downstream shielding plates

301A, 301B, and 301C as described above, it is possible to more effectively suppress the temperature drop inside the inner cylindrical body 21.

According to the second embodiment described above, in addition to the effects [1] to [5] of the first embodiment, the following effects can be obtained.
[6] Since the downstream shielding member 30A is composed of a plurality of

downstream shielding plates

301A, 301B, 301C, the probability that the organic EL element material comes into contact with the inner wall of the inner cylinder 21 is increased, and the yield is improved. In addition, it is possible to more effectively suppress the temperature drop at the end inside the inner cylinder 21.
Therefore, since the temperature drop in the collector can be suppressed and the purity of the sublimate recovered can be increased, the yield of the organic EL element material recovered on the inner wall 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.

The shape of the apparatus main body of the present invention is not particularly limited.
For example, the shape, number, and size of the through hole 272D in the downstream shielding plate 271D are not limited to those illustrated in FIG. The shape of the through hole 272D may be an arbitrary shape such as a quadrangle or other polygons. Further, as shown in FIG. 5, the through hole 272D may be a downstream shielding plate 271C having a through hole 272C surrounded by a straight line connecting the arc and its end.

Furthermore, as shown in FIG. 6, instead of the

downstream shielding plates

301A, 301B, 301C in the second embodiment, a downstream shielding member 30B may be provided using a plurality of downstream shielding plates 271C. In this case, the downstream shielding plates 271C are arranged so as to be out of phase so that the through holes 272C of the adjacent downstream shielding plates 271C do not overlap when viewed from the thickness direction of the downstream shielding plates 271C. By providing the downstream shielding plate 271C in this manner, the airflow including the organic EL element material passes through the downstream shielding member 30B while meandering.
Further, as shown in FIG. 7, the downstream shielding member 30A of the second embodiment is a downstream shielding member 30C provided with an opening by a downstream shielding plate 271F formed by cutting off a part of a circular arc of a circular plate. It is good.

Further, the downstream shielding member 30A may be configured as shown in FIG.
In the downstream shielding member 30E shown in FIG. 8,

downstream shielding plates

271K, 271L, and 271M are arranged in this order as the

downstream shielding plates

301A, 301B, and 301C. The through holes 272K of the downstream shielding plate 271K, the through holes 272L of the downstream shielding plate 271L, and the through holes 272M of the downstream shielding plate 271M have fan shapes with different opening areas, and are viewed from the thickness direction of the

downstream shielding plates

271K, 271L, 271M. The through

holes

272K, 272L, and 272M are provided with a phase shift so that they do not overlap.

In the second embodiment, the three

downstream shielding plates

301A, 301B, and 301C are used. However, the number of downstream shielding plates may be two, or four or more.
Furthermore, instead of the downstream shielding plate 271D in the first embodiment, the

downstream shielding plates

271C, 271F, 271K, 271L, and 271M may be used alone.

In the above embodiment, instead of providing the end shielding member 28 constituted by one end shielding plate 281, an end shielding member 30 constituted by three end shielding plates 281 may be provided. FIG. 9 shows a plan view of the end shielding member 30. The end shielding member 30 includes three

end shielding plates

311A, 311B, and 311C, and each of the

end shielding plates

311A, 311B, and 311C has a plurality of through holes 312A that are provided radially from the center. 312B and 312C. The three

end shielding plates

311A, 311B, and 311C are all the same as the end shielding plate 281 and the through

holes

312A, 312B, and 312C are the same as the through hole 282. The end shielding member 30 is configured such that these

end shielding plates

311A, 311B, 311C are spaced apart from each other by a predetermined distance and the phase of the second end shielding plate 311B is shifted. In the end shielding member 30, the through

holes

312A, 312B, 312C are openings, and portions other than the through

holes

312A, 312B, 312C are closed portions.
As described above, by configuring the end shielding member 30 with the plurality of

end shielding plates

311A, 311B, 311C, it is possible to more effectively suppress the temperature drop inside the inner cylindrical body 21.

As shown in FIG. 10, the end shielding member 30 is adjacent to the

end shielding plates

311A, 311B, 311C when viewed from the direction (thickness direction) orthogonal to the

end shielding plates

311A, 311B, 311C. The through

holes

312A, 312B, 312C of the matching end shield plates are provided so as not to overlap. That is, the through hole 312A and the through hole 312B are provided so that the through hole 312B and the through hole 312C do not overlap.

When the through

holes

312A, 312B, and 312C are formed in this way, as shown by arrows in FIG. 10, the airflow including the organic EL element material passes through the through hole 312A and comes into contact with the end shielding plate 311B. Bends and passes through the through hole 312B. Then, it comes into contact with the end shielding plate 311C, bends again, and passes through the through hole 312C. As described above, when the air flow including the organic EL element material passes through the through

holes

312A, 312B, and 312C in a meandering manner without going straight through the end shielding member 30, the

end shielding plates

311A, 311B, and 311C It collides with the closed part, making it difficult for heat to escape downstream. Accordingly, the temperature inside the inner cylinder 21 can be suppressed from decreasing, and the probability that the organic EL element material and the inner wall are in contact with each other is increased, so that the yield of the organic EL element material collected on the inner wall is improved. Can do.

Further, the shape, number and size of the through holes 282 in the end shielding plate 281 are not limited to those shown in FIG. As shown in FIG. 11, it is good also as an end part shielding board 281A which has the circular through-hole 282A which has a large diameter gradually from a center part. Moreover, as shown in FIG. 12, it is good also as the edge part shielding board 281B which has arrange | positioned the through-hole 282B in the outer periphery side of a shielding board, and made a part of through-hole 282B into a different size.

Further, the end shielding member 30 may be an end shielding member 30D shown in FIG. An end shielding member 30D shown in FIG. 13 is configured by arranging

end shielding plates

281G, 281H, and 281J in this order as

end shielding plates

311A, 311B, and 311C. The through-hole 282G of the end shield plate 281G, the through-hole 282H of the end shield plate 281H, and the through-hole 282J of the end shield plate 281J are circular in diameter in this order, and the

end shield plates

281G, 281H, 281J. When viewed from the thickness direction, the through

holes

282G, 282H, 282J are provided with a phase shift so that they do not overlap.

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.

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. Examples include stainless steel, tantalum, tungsten, molybdenum, titanium, zirconia, carbon, alumina, boron nitride, silicon nitride, and Teflon (registered trademark).
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 above-described embodiment, the second inner cylinder 61 of the collector 6 is described as being divided into three collection chambers R1, R2, and R3. However, 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.

The setting of the heating temperature for each collection chamber R1, R2, R3 of the collector 6 is not limited to that described in the above embodiment. For example, the first collection chamber R1 is heated and held lower than the condensation temperature of the organic EL element material to be purified, the second collection chamber R2 is heated and held at the same temperature, and the third collection chamber R3 may be heated and held higher.

In the above embodiment, the powdery organic EL element material is accommodated in the accommodating part 54 and evaporated to be purified, but the liquid organic EL element material is accommodated in the accommodating part 54 and vaporized. And may be purified.
The organic material refine | purified with the refiner | purifier 1 of this invention is not limited to an organic EL element material. Moreover, the organic material refine | purified with the refiner | purifier 1 of this invention may be refine | purified repeatedly, and purity may be raised further.

Next, the present invention will be described in more detail with reference to examples and comparative examples, but the present invention is not limited to these examples.

[Example 1]
(Purification equipment)
A purifier with only a downstream shielding member was used. The collector was divided into five, and sampling was performed at points S1 to S5. The points S1 to S5 are located in the order of S1, S2, S3, S4, and S5 from the upstream side of the collector 6. The inner cylinder of the refining device is made of quartz, and the downstream shielding member is made of stainless steel.
(Purification of materials for organic EL devices)
This organic EL element material was put in a housing portion, the heater and the temperature adjusting heater were heated, and the organic EL element material was purified.

[Comparative Example 1]
In Example 1, a downstream shielding member was not provided, and the organic EL element material was purified in the same manner as in Example 1.

The organic EL device material purified in Example 1 and Comparative Example 1 was sampled at each point S1 to S5, and the yield and purity were measured at each point S1 to S5.

In Example 1, the organic EL device material having a certain purity or higher that can be used as a product was recovered at all points S1 to S5.
On the other hand, in Comparative Example 1, the purity of the organic EL element material at points S4 and S5 is lower than a certain purity that can be used as a product, and the organic EL element material recovered at points S4 and S5 The purity was not reached.
As for the total yield of organic EL element materials having a certain purity or higher that can be used as a product, Example 1 was 7% higher than Comparative Example 1.
In Comparative Example 1, the purity of the organic EL element material collected at points S4 and S5 was low because the downstream shielding member was not provided, so the temperature drop inside the inner cylinder at the points S4 and S5 This is probably because impurities that have a sublimation temperature lower than that of the organic EL material to be purified are also collected. In addition, the temperature difference between Example 1 and Comparative Example 1 at points S4 and S5 was 20 ° C. at point S4 and 50 ° C. at point S5.

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

1 ... Purification device 3 ... Vacuum pump (exhaust device)
DESCRIPTION OF SYMBOLS 5 ... Vaporizer 6 ... Collector 25 ... Shielding part 26 ... Upstream shielding

member

27, 30A, 30B ... Downstream shielding

member

28, 30 ... End part shielding member 51 ... First inner cylinder (first cylinder)
53 ... Heater 54 ... Housing (raw material container)
61 ... Second inner cylinder (second cylinder)
63 ... Temperature adjustment heater 261 ...

Upstream shielding plate

271C, 271D, 271E, 271F, 271G, 271K, 271L, 271M, 301A, 301B, 301C ...

Downstream shielding plate

272C, 272D, 272K, 272L, 272M, 282,282A, 282B , 282G, 282H, 282J, 302A, 302B, 302C, 312A, 312B, 312C ... through hole (opening)

Claims

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 wall of the second cylinder;
An exhaust device connected downstream of the collector;
An organic material comprising: a shielding member provided at both ends of an inner cylinder formed by communicating the first cylinder and the second cylinder, and having an opening and a closing part. Purification equipment.
In the refiner | purifier of the organic material of Claim 1,
An outer cylinder that houses the inner cylinder;
The organic material refinement | purification apparatus characterized by further providing the said shielding member in the both ends of the said outer cylinder.
In the refiner | purifier of the organic material of Claim 1 or Claim 2,
The organic material purifier according to claim 1, wherein an area ratio between the opening and the blocking portion in the shielding member is 5:95 to 50:50.
In the refiner | purifier of the organic material of Claim 2 or Claim 3,
The opening of the shielding member of the outer cylinder is formed with a plurality of through holes radially from the central portion of the shielding member,
The organic material refining device, wherein the opening of the shielding member of the inner cylindrical body is formed with a through hole having a shape surrounded by a circle or a circular arc and a straight line connecting both ends of the circular arc.
In the refiner | purifier of the organic material as described in any one of Claims 1-4,
The shielding member includes a plurality of shielding plates arranged apart from each other.
Each of the plurality of shielding plates includes the opening,
The organic material refining device, wherein the openings of adjacent shielding plates do not overlap when the shielding plates are viewed from an orthogonal direction.
In the refiner | purifier of the organic material as described in any one of Claims 1-5,
A raw material container to which the organic material is supplied is installed inside the first cylindrical body,
In the inner cylinder, the shielding member installed at the end of the first cylinder opposite to the side communicating with the second cylinder and upstream of the raw material container has an opening. Organic material refining equipment characterized by not having.