KR20130049935A - Tube for sublimation purifying - Google Patents

Tube for sublimation purifying Download PDF

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Publication number
KR20130049935A
KR20130049935A KR1020110114995A KR20110114995A KR20130049935A KR 20130049935 A KR20130049935 A KR 20130049935A KR 1020110114995 A KR1020110114995 A KR 1020110114995A KR 20110114995 A KR20110114995 A KR 20110114995A KR 20130049935 A KR20130049935 A KR 20130049935A
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KR
South Korea
Prior art keywords
tube
diameter
sublimation
inner tube
organic material
Prior art date
Application number
KR1020110114995A
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Korean (ko)
Inventor
황순규
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황순규
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Application filed by 황순규 filed Critical 황순규
Priority to KR1020110114995A priority Critical patent/KR20130049935A/en
Publication of KR20130049935A publication Critical patent/KR20130049935A/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D7/00—Sublimation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B63/00—Purification; Separation; Stabilisation; Use of additives

Abstract

PURPOSE: A shell for sublimation purification is provided to increase yield and productivity of organic crystalline and to accept samples without using a boat. CONSTITUTION: A shell for sublimation purification is a shell of an inner pipe in which organic material samples among inner pipes which are arranged in many rows in a longitudinal direction of an outer pipe by being adopted to the outer pipe equipped in the sublimation purification device. The shell for the sublimation purification has a cylindrical shape, and a first diameter (111) of one end is sealed and a second diameter (112) of the other end is opened. The second diameter is processed to be smaller than the first diameter by making a steep surface (121) from one region to the second diameter direction.

Description

Tube for sublimation purifying

The present invention relates to a sublimation tablet tube, and more particularly, to the organic EL device or AMOLED used in the organic EL device or AMOLED so that the yield and productivity of the organic crystal can be increased while the loss of the organic material is minimized. The present invention relates to a sublimation tablet tube having a double pipe connection structure applied to a conventional sublimation tablet device for sublimation purification.

The sublimation purification tube replaces the inner tube in which the organic material sample is accommodated among the inner tubes provided in the sublimation purification apparatus.

The organic EL device is composed of several thin organic thin film layers between a cathode having a large work function and a transparent anode and a cathode having a low work function.The principle of emission is to inject holes into the organic layer from the anode electrode when a voltage is applied to the device in the forward direction. Is a display device in which electrons are injected to recombine in the emission layer to emit light.

The organic EL device has all of the high quality panel characteristics required in the information age such as low power consumption, wide viewing angle, high speed response speed, and wide driving temperature range, and also has a relatively simple manufacturing process to transcend conventional flat panel displays. It has the advantage that can be expected to realize low price.

Purity of the organic material is a factor influencing the light emission characteristics of the organic EL device as described above. If impurities are mixed in the organic material, the impurities become traps of carriers or cause quenching, and the emission intensity and luminous efficiency are lowered. Therefore, it is necessary to purify organic materials to reduce impurities.

As a purification method of such an organic material, recrystallization using a solvent or recrystallization by sublimation is generally used. Recrystallization using a solvent has the advantage that it is possible to purify the organic material in large quantities, but since the solvent is used, the solvent tends to enter the organic crystals. The solvent that enters into the organic crystal can act as an impurity and lower the luminescence properties.

On the other hand, in recrystallization by sublimation, impurities are less likely to enter since organic materials are sublimed and recrystallized under vacuum. Therefore, the sublimation purification method is mainly used for the purification of the organic material for EL elements.

H. J. Wagner, el al., Jounal of Materials Science, 17, 2781, (1982) discloses a sublimation purification apparatus for organic materials. In the sublimation refining apparatus disclosed in the above paper, a glass tube having a length of about 1 m is inserted into a copper tube for heat conduction, and a sample of an organic material to be purified is disposed in one end region of the glass tube. A heater is attached to surround the copper tube around the organic material sample, and the inside of the glass tube is maintained in a vacuum state of about 200 Pa, and the sample in the glass tube is heated by the heater to sublimate the organic molecules of the sample. The glass tube is temperature-graded and the vapor of organic molecules is cooled and recrystallized in the other end region of the glass tube. This produces recrystallized organic crystals in the other end region of the glass tube.

FIG. 1 is a schematic and partial enlarged view of a conventional sublimation purification apparatus for organic materials, wherein inner tubes 20 are arranged inside an outer tube 10 having a predetermined length, and the inner tube 20 The heaters 30 are connected to each other through the connection member 25, and a plurality of heaters 30 are arranged outside the outer tube 10.

At this time, the inner tube 20 in which the organic material sample 23 of the inner tube 20 is accommodated in the boat pedestal for placing the organic material boat 21 and the organic material boat 21 in the inner tube 20 ( 22) is configured.

In the conventional sublimation purification apparatus to which the organic matter boat 21 is applied as described above, when the organic material boat 23 is accommodated in the organic matter boat 21, the sublimation purification may be performed. There is a problem that the loss of organic material is a lot, the yield of organic crystals are lowered and productivity is lowered as a process of being polluted to the bottom of the organic material boat 21 and discarded through denaturation occurs.

Accordingly, the present invention has been made to solve the above conventional problems, the object of the present invention is applied to a conventional sublimation purification device for the sublimation purification of organic materials used in organic EL devices or AMOLED (AMOLED) It is to provide a sublimation purification tube that can increase the yield and productivity of organic crystals.

In addition, another object of the present invention is applied to a conventional sublimation retention device As a body , Open At one end  Sublimation tablets, which allow processing of samples on their own without the use of boats by allowing them to be processed in a narrower direction Tube  To provide.

In addition, another object of the present invention is a tube body to be applied to a conventional sublimation purification device, the inner tube and the outer tube is formed in the form of a double tube connection structure to replace the inner tube in which the organic material sample of the inner tube is accommodated The present invention provides a sublimation and purification tube having a structure that minimizes the loss of organic materials during sublimation purification by utilizing the inside of the inner tube as a space for receiving an organic material sample.

In addition, another object of the present invention is to connect the funnel-shaped acceleration tube without a connecting member to the next stage of the tube of the double connection and structure, the material of the organic material sublimated by heating in the tube of the double connector structure is accelerated It is to provide a sublimation refining tube with a structure that can be accelerated as it passes through to produce a lot of purified products. Here, the funnel-shaped acceleration tube serves to improve the inefficiency that the material of the sublimed organic material is slow and does not reach the last tube, but falls into the middle tube, thereby reducing the productivity of the purified product.

The present invention for achieving the above object, in the sublimation purification device,

A tube structure of an inner tube accommodated in an outer tube provided in the sublimation purification apparatus and containing a sample of organic material among inner tubes disposed in a plurality of rows in the longitudinal direction of the outer tube, wherein the tube is formed by The first diameter is sealed, and the cylindrical shape having a structure in which the second diameter of the other end is open, the inclined surface in the direction of the second diameter from one region is processed so that the second diameter is smaller than the first diameter Disclosed is a sublimation purification tube.

In addition, in the sublimation purification apparatus, a pipe structure of an inner tube which is housed inside the outer tube provided in the sublimation purification apparatus and accommodates samples of organic materials among the inner tubes disposed in a plurality of rows in the longitudinal direction of the outer tube. The tubular body may include a cylindrical inner tube having a structure in which one end of the first diameter is sealed and the second end of the other is partially open; And a cylindrical shape accommodating the inner tube therein, the inclined surface having a length toward the other end side of the second diameter of the inner tube so that the inclined surface is hermetically coupled to the outer diameter of the inner tube, and the inner tube is accommodated therein. A sublimation and purification pipe body characterized in that it is formed in a double-connected tube structure; an outer tube forming a plurality of supports connected to the outer diameter of one end of the first diameter of the inner tube so that the horizontal can be maintained in the It starts.

Preferably, the opening of the second diameter formed at the other end of the inner tube is configured such that the upper part of the diameter is opened in the range of 25 to 75% in proportion to the size of the diameter according to the properties of the organic material for the sublimation tablet. Can be.

Preferably, the plurality of supports is more preferably at least three or more for stable horizontal maintenance of the inner tube accommodated therein.

Preferably, the outer tube is heated by the heater to evenly heat the inner tube through the open space on the side where the support is formed, and the inner end of the housing formed with the support is extended so as to extend for a long time to stay inside It is more preferable to form.

In addition, the next stage of the tube is connected to the inclined surface of the outer tube without a connecting member to form a funnel-shaped acceleration tube for accelerating the sublimation of the organic material during the sublimation purification process; The material of the sublimed organic material exothermic at is passed through the acceleration tube to be accelerated more rapidly to produce a large amount of purified products.

As described above, according to the sublimation purification tube according to the present invention, in the conventional sublimation purification apparatus used for the sublimation purification of organic materials, the inner tube and the outer tube are formed in the form of the connection structure of the double tube. When applied as an inner tube to accommodate a material sample, it minimizes the loss of organic materials as compared to the inner tube using an organic boat, and provides the effect of maximizing productivity of high-purity organic crystals with high yield.

In the case of the inner pipe using the existing organic material boat, this prevents the problem that organic material that is not moved through sublimation is contaminated at the bottom of the organic water boat and is contaminated and discarded through denaturation. Done.

In addition, the present invention is to provide a sublimation and purification pipe body that can be accommodated by the sample itself without using a boat by processing in the direction that the diameter of the open end of the tube is gradually narrowed.

In addition, the present invention can reduce the number of sublimation purification to obtain a high-purity organic crystal of high yield, which provides the effect of reducing the manufacturing cost.

In addition, the present invention by placing a funnel-shaped acceleration tube that can be connected without a connecting member to the next stage of the tube of the double connection and structure, the material of the organic material sublimated by heating in the tube of the double connector structure passes through the acceleration tube It provides an effect that allows for much faster purification with the faster acceleration.

That is, the funnel-shaped acceleration tube improves the inefficiency that the material of the sublimed organic material is slow and does not reach the last tube, but falls to the middle tube, thereby reducing the productivity of the purification result.

1 is a schematic diagram and a partially enlarged view of a conventional sublimation purification apparatus for organic materials;
Figure 2 is a perspective view and a cross-sectional view shown for explaining the sublimation tablet tube according to an embodiment of the present invention,
3 is a reference diagram shown to explain the opening of the inlet side diameter of the inner tube of the sublimation tablet pipe according to FIG.
Figure 4 is a reference diagram showing the cross section AA of the sublimation tablet tube according to Figure 2,
Figure 5 is a cross-sectional view shown for explaining an example of the sublimation tablet tube according to the present invention,
5 is a reference diagram shown to explain the connection process of the sublimation purification tube according to the invention, and
6 is a schematic view showing a sublimation purification apparatus of an organic material to which the sublimation purification tube according to the present invention is applied.

Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear.

Figure 2 is a perspective view and a cross-sectional view shown for explaining the sublimation tablet pipe according to an embodiment of the present invention, Figure 3 is a reference shown to explain the opening of the inlet side diameter of the inner tube of the sublimation tablet pipe according to Figure 2 FIG. 4 is a reference view showing an AA cross section of the sublimation tablet tube according to FIG. 2.

As shown, the sublimation tablet tube according to an embodiment of the present invention, the inner tube 110 and the outer tube 120 has a double tube structure having a double tube structure.

At this time, the tubular body 100, as shown in Figure 1, is accommodated in the interior of the outer tube 10 provided in the conventional sublimation purification apparatus is disposed in a plurality of rows in the longitudinal direction of the outer tube 10 Of the tubes 20 is a structure that can be configured to replace the inner tube 20, the sample 23 of the organic material is accommodated.

As shown, the inner tube 110 of the tubular body 100 has a cylindrical structure having a structure in which one end of the first diameter 111 is sealed through a seal and the second diameter 112 of the other end is partially opened. Is formed.

As illustrated, the outer tube 120 of the tubular body 100 has a cylindrical shape accommodated therein in a form of surrounding the inner tube 110 with a space outside thereof, and has a second diameter of the inner tube 110. An inclined surface 121 having a length is formed on the other end side of the 112, and an end of the inclined surface 121 is sealed to the outer diameter 113 of the inner tube 110.

In addition, the outer tube 120 has one end of the first diameter 111 of the inner tube 110 through the plurality of supports 122 so that the inner tube 110 is horizontally maintained in a state accommodated therein. Connect with the outer diameter 113 of.

Accordingly, the tubular body 100 constitutes a double connecting tube structure in which the inner tube 110 and the outer tube 120 are composed of one inner tube, and the tubular body 100 is the inside of a conventional sublimation purification apparatus. The tube may be replaced and applied as a tube for receiving a sample of organic material.

The shape of the tubular body 100 as described above minimizes the loss of the organic material, as well as high purity, compared to the conventional case of sublimation purification by placing the sample 23 of the organic material in a separate organic material boat 21. This provides the advantage of obtaining organic crystals.

In particular, in the case of the inner tube 20 using the conventional organic material boat 21, the organic material that is not moved through the sublimation falls to the bottom of the organic material boat 21 is contaminated and is discarded through denaturation As a result, the yield of organic crystals may decrease and productivity may decrease.

On the contrary, the tubular body 100 of the present invention prevents the loss of organic materials by directly utilizing the inside of the inner tube 110 composed of the double tube as a space in which the organic material sample 23 is accommodated, and the productivity of organic crystals. It will provide an advantage that can be increased.

In addition, the opening of the second diameter 112 formed at the other end of the inner tube 110 of the double tube of the tubular body 100, as shown in Figure 3, the upper part of the diameter according to the characteristics of the organic material for the sublimation tablet It is configured to open in the range of 25 to 75% in proportion to the size of the diameter.

In addition, as shown in FIG. 4, the plurality of supports 122 are formed to be connected to at least three or more for stable horizontal maintenance of the inner tube 110 accommodated in the outer tube 120. . This prevents the organic material sample 23 in the inner tube 110 from flowing out through the stable horizontal maintenance of the inner tube 110 during the sublimation purification process.

4 (a) shows three supports 122, and FIG. 4 (b) shows four supports 122. As shown in FIG. The support 122 is not limited to the number and can be formed even more, it should be understood that any shape as long as it is a function for maintaining the horizontal center of the inner tube (110).

In addition, the outer tube 120 is heated so that the air warmed by the heater 30 evenly heats the inner tube 110 through the open space on the side where the support 122 is formed, and stays therein for a long time. The housing end 123 on which the support 122 is formed is formed to be bent and extended in about 2 cm.

As shown in FIG. 1, in the related art, the temperature warmed when the organic material sample 23 is placed in the boat 21 is directly in contact with the organic material sample 23. And the temperature difference is generated at the top, but in the present invention by forming the housing end 123 to be bent to extend, the air warmed by the heater 30 is introduced through the open space evenly to the inner tube 110 At the same time as the heating to prevent the warm air flowing into the inside to be easily leaked to the outside. Through this, the temperature for sublimation of the organic material sample 23 can be more stably maintained.

On the other hand, the tube 100 is not limited to the double tube 100 as shown in Figures 2 to 4, for example, the diameter of the tube 100 is approximately 250 to 300mm or more in diameter, or the inclined surface 121 According to the angle adjustment of) may be one independent tube, which will be described with reference to FIG.

5 is a cross-sectional view illustrating an example of a sublimation tablet tube according to the present invention.

As shown, the tubular body 100 is an independent tubular body, in which the first diameter 111 is closed and the second diameter 112 is fully open. In this case, the organic material sample 23 is disposed therein. It is accommodated, but is supported on the inside of the inclined surface 121 is prevented from being separated from the tube body (100).

That is, since the height value of the inclined surface 121 increases as the tube 100 is enlarged as shown in FIG. 5A, the organic material sample 23 can be prevented from being separated from the tube 100, and as shown in FIG. 5B. Irrespective of the diameter of the tubular body 100, the organic material sample 23 can be prevented from being separated from the tubular body 100 by the inclined surface 121 by adjusting the angle of the inclined surface 121.

FIG. 6 is a reference diagram illustrating a connection process of a sublimation purification tube according to the present invention, and FIG. 7 is a schematic view illustrating a sublimation purification apparatus of an organic material to which a sublimation purification tube according to the present invention is applied. .

6 and 7, the next stage of the tubular body 100 is coupled to the inclined surface 121 of the outer tube 120 without the connecting member 25 to sublimate the organic material during the sublimation purification process. It may be configured to further include an acceleration tube 200 for accelerating.

The acceleration tube 200 has a connection structure corresponding to the shape of the tube 100, and serves to increase the flow rate of the sublimated organic material by Bernoulli theory that the flow rate increases as the inlet is narrowed. .

That is, the acceleration tube 200 is a funnel shape of the overall shape of the heat pipe in the double-connected tube structure 100, the material of the sublimed organic material passes through the narrowing tube of the acceleration tube 200 a little faster By accelerating to reach the last tube stably, the result is a large amount of organic material purification results.

This results in the purification resulted from the tubular body 100 of the double-connected tube structure, and the sublimed material does not reach the last tube (# 5) 20 but falls off to the intermediate tube (# 3, # 4) 20. This diminishing inefficiency will be improved.

While the present invention has been particularly shown and described with reference to exemplary embodiments thereof, it is to be understood that the invention is not limited to the disclosed exemplary embodiments.

10: outer tube 20: inner tube
21: Organics Boat 22: Boat Pedestal
23: organic material sample 24: organic crystal
25: connecting member
100: tube 110: inner tube
111: first diameter 112: second diameter
113: outer diameter 120: outer tube
121: inclined surface 122: support
123: housing end 200: acceleration tube

Claims (6)

In the sublimation purification device,
A tube structure of an inner tube accommodated in an outer tube provided in the sublimation purification apparatus and containing a sample of an organic material among inner tubes disposed in a plurality of rows in the longitudinal direction of the outer tube, wherein the tube is
One end of the first diameter is sealed, the second diameter of the other end of the cylindrical shape having an open structure, the inclined surface in the direction of the second diameter from one region is processed so that the second diameter is smaller than the first diameter. Sublimation tablet pipe. In the sublimation purification device,
A tube structure of an inner tube accommodated in an outer tube provided in the sublimation purification apparatus and containing a sample of an organic material among inner tubes disposed in a plurality of rows in the longitudinal direction of the outer tube, wherein the tube is
A cylindrical inner tube having a structure in which one end of the first diameter is sealed and the second diameter of the other end is partially open; And
A cylindrical shape accommodating the inner tube therein, and forms an inclined surface having a length to the other end side of the second diameter of the inner tube so that the inclined surface is sealingly coupled to the outer diameter of the inner tube, the inner tube is accommodated therein Sublimation and purification pipe body, characterized in that formed in a double-connected tube structure; an outer tube forming a plurality of supports connected to the outer diameter of one end of the first diameter of the inner tube so that the horizontal can be maintained. The method of claim 2,
The opening of the second diameter formed at the other end of the inner tube,
Sublimation tablet tube according to the characteristics of the organic material for sublimation purification characterized in that the upper portion of the diameter is configured to open in the range of 25 to 75% in proportion to the size of the diameter. The method of claim 2,
The plurality of supports,
Sublimation and purification pipe body, characterized in that at least three or more for stable horizontal maintenance of the inner tube accommodated in the interior. The method of claim 2,
The outer tube,
Sublimation tablets characterized in that the air warmed by the heater to evenly heat the inner tube through the open space on the side where the support is formed, and to extend the end of the housing formed with the support so that it can stay for a long time inside Dragon tube. The method of claim 2,
Next to the tube is a funnel-shaped acceleration tube for accelerating the sublimation of the organic material during the sublimation purification process is fastened to the inclined surface of the outer tube without a connecting member; thereby, generating heat in the tube of the double connector structure Sublimation purification tube characterized in that the material of the sublimed organic material is subjected to a faster acceleration while passing through the acceleration tube to produce a large amount of purified product.
KR1020110114995A 2011-11-07 2011-11-07 Tube for sublimation purifying KR20130049935A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20150064501A (en) * 2013-12-03 2015-06-11 주식회사 엘지화학 Sublimation refining apparatus and sublimation refining method using the same
KR102176768B1 (en) * 2020-01-28 2020-11-10 정훈도 Sublimation purification apparatus and method

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20150064501A (en) * 2013-12-03 2015-06-11 주식회사 엘지화학 Sublimation refining apparatus and sublimation refining method using the same
KR102176768B1 (en) * 2020-01-28 2020-11-10 정훈도 Sublimation purification apparatus and method

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