KR20150094009A - Apparatus for low temperature sublimation purification - Google Patents

Abstract

The present invention relates to a sublimation purification apparatus at low temperatures, for purifying a material sublimated at low temperatures. According to an embodiment of the present invention, provided is a sublimation purification apparatus at low temperatures, which comprises: a base frame; an outer tube having one side settled on the upper side of the base frame; an inner tube inserted to the inside of the outer tube; a cover coupled with the upper part of the base frame; and a heater equipped on the base frame or the inside of the cover, wherein the other side of the outer tube extended to the outside of the base frame is coupled with at least one cooling jacket.

Description

[0001] APPARATUS FOR LOW TEMPERATURE SUBLIMATION PURIFICATION [0002]

The present invention relates to an apparatus for sublimating and purifying impurities using a temperature change temperature of a material, and more particularly, to a low temperature sublimation purification apparatus for purifying a material that sublimates at a low temperature.

The organic material is usually purified using a sublimation purification method. Sublimation refers to the gas-solid transition occurring at temperatures and pressures below the triple point in the phase equilibrium, and even if the material is pyrolyzed by heating at normal pressure, it does not decompose even at relatively low temperatures at low pressures below the triple point State is maintained.

Utilizing this property, in the sublimation apparatus capable of controlling the temperature gradient, an operation in which the synthesized substance is heated to separate the sublimation point from the other sublimation state without decomposition is referred to as a vacuum sublimation method.

Such a vacuum sublimation method is a pure physical method because it does not depend on the use of auxiliary reagents or other chemical methods, and therefore has no advantage of contamination by the sample and has a large separation rate, and is a useful method for purifying organic materials for organic electroluminescence devices .

An apparatus for performing such a vacuum sublimation method is disclosed in Korean Patent No. 10-0582663 (Patent Document 1) and the like, and FIG. 1 is a view schematically showing such a vacuum sublimation apparatus.

In this case, the material to be purified is contained in a quartz or glass refining tube 4, and the refining tube 4 is disposed on one side of the inner tube 1. The inner tube 1 is interconnected by a connecting member 3 and the outer tube 2 surrounds the outer side of the inner tube 1. The heater 5 is installed so as to surround one side of the outer tube 2. The place where the heater 5 is disposed corresponds to the position where the refining tube 4 is disposed. On the other hand, the vacuum pump 6 is disposed on the other side of the inner tube 1 to evacuate the inside of the inner tube 1.

At this time, when the temperature is gradually increased by using the heater 5, a temperature gradient is formed over the entire inner tube 1. When the temperature of the refining tube 4 becomes higher than the sublimation point of the material to be refined contained therein, The material sublimes and starts to move toward the vacuum pump 6 in the form of gas molecules, and the impurities remain in the interior of the purifying tube 4.

The sublimated and moved gas molecules are transferred to the solid phase again in the section of the inner tube 1 having a temperature lower than the sublimation point and are made into a crystalline state on the inner peripheral surface of the inner tube 1. After a sufficient time has elapsed, heating is stopped The inner tube 1 is disassembled and the purified material 25 in the crystalline state is scraped off and recovered.

In order to crystallize the refining material 25, it is necessary to control the specific section of the inner tube 1 to a temperature lower than the sublimation temperature of the material. Normally, by controlling the temperature of the heater 5, Section is controlled to the acquisition temperature of the refining material.

On the other hand, the principle of this vacuum sublimation method can be applied to a material which is purified by a conventional chemical purification process (column). However, these materials have a generally low sublimation temperature, and conventional sublimation purification apparatuses obtain a sublimation material at a low temperature (for example, an intermediate of the pre-synthesis step of the compound, for example, 8-hydroxyninoline) It is not suitable for the following.

For example, in the case of a refining material which is sublimated at about 50 캜 and crystallized at a temperature of 20 캜 or lower, as the material sublimated by heating moves with heat, a section for obtaining the refining material is affected by heat transfer , It becomes impossible to realize the target crystallization temperature.

Therefore, in order to eliminate the thermal influence, it is necessary that the acquisition section for acquiring the refining material is located far away from the vaporizing section where the heater is disposed. In this case, the electric field of the sublimation refiner becomes long, There is a problem that the installation cost is increased, and the sublimation purification time is further increased, resulting in a problem that the productivity is lowered.

In addition, since the environmental conditions of the clean room for installing the sublimation refining apparatus are generally controlled at 20 ° C to 27 ° C, depending on the method of using a heater or increasing the total length of the apparatus, Can not be controlled below 20 [deg.] C, which is lower than the ambient temperature of the clean room.

KR 10-0582663 B1 (May 16, 2006 Enrollment)

SUMMARY OF THE INVENTION The present invention has been conceived in order to solve the problems as described above. One embodiment of the present invention is to provide a method of manufacturing a semiconductor device, which is capable of purifying a material in which sublimation occurs at a low temperature, It is an object of the present invention to provide a sublimation purification apparatus.

According to a preferred embodiment of the present invention, a base frame, An outer tube having one side seated on the upper side of the base frame; An inner tube inserted into the outer tube; A cover coupled to an upper portion of the base frame; And a heater provided on the inner side of the base frame or the cover, wherein at least one cooling jacket is coupled to the other side of the outer tube extending outside the base frame. do.

Here, a plurality of cooling jackets are coupled to the other side of the outer tube so that a low temperature temperature gradient is formed inside the inner tube extending outside the base frame.

At this time, at least one pair of the plurality of cooling jackets is supplied with a refrigerant at a different temperature.

The cooling jacket may include a hollow tube coupled to an outer circumferential surface of the outer tube so as to surround the outer tube.

The cooling jacket is preferably made of a transparent material so that the state of the sample to be obtained can be confirmed.

In order to supply the coolant to the cooling jacket, a coolant supply device is provided on one side of the base frame.

The cooling jacket is made of a transparent material, and a color dye may be added to the refrigerant supplied to the cooling jacket in order to block light.

At this time, the refrigerant supply device includes a refrigerant supply pump installed at one side of the base frame, a supply pipe connected to supply the refrigerant from the refrigerant supply pump to the cooling jacket, And a discharge pipe connected to discharge the gas.

Meanwhile, the cooling jacket may include a metal case coupled to surround the outer tube, and at least one cooling line provided inside the case.

At this time, a viewport window is provided on one side of the case so that the state of the acquired sample can be confirmed.

In addition, a heat insulating coating layer may be formed on the inner surface of the cooling jacket.

According to the low-temperature sublimation refining apparatus according to the embodiment of the present invention, the section for controlling the temperature of the acquisition section to a low temperature by the cooling jacket and sublimating the material is separately constituted, so that the sublimation purification for the material having the low- .

In addition, since a low temperature temperature gradient can be formed by a plurality of cooling jackets, it is easy to separate and obtain the refined material and the impurity from the sublimated material.

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a schematic diagram schematically illustrating a conventional vacuum sublimation apparatus. Fig.
2 is a schematic diagram of a low temperature sublimation purification apparatus according to an embodiment of the present invention.
3 is a cross-sectional view of a cooling jacket according to an embodiment of the present invention.
4 is a longitudinal sectional view of a cooling jacket according to an embodiment of the present invention;
FIG. 5 is a schematic view illustrating a vaporizing unit and an obtaining unit according to an embodiment of the present invention; FIG.

Hereinafter, preferred embodiments of the low temperature sublimation purification apparatus of the present invention will be described with reference to the accompanying drawings. In this process, the thicknesses of the lines and the sizes of the components shown in the drawings may be exaggerated for clarity and convenience of explanation.

In addition, the terms described below are defined in consideration of the functions of the present invention, which may vary depending on the intention or custom of the user, the operator. Therefore, definitions of these terms should be made based on the contents throughout this specification.

In addition, the following embodiments are not intended to limit the scope of the present invention, but merely as exemplifications of the constituent elements set forth in the claims of the present invention, and are included in technical ideas throughout the specification of the present invention, Embodiments that include components replaceable as equivalents in the elements may be included within the scope of the present invention.

Example

2 is a schematic view of a low temperature sublimation purification apparatus according to an embodiment of the present invention.

2, a low temperature sublimation purification apparatus 100 according to an embodiment of the present invention includes a base frame 200, An inner tube 400 (see FIG. 3) inserted into the outer tube 300; a cover 500 hinged to the upper portion of the base frame 200; And a heater 600 disposed inside the cover 200 or the cover 500.

Here, the base frame 200 may be installed on the table 900, for example, as shown in FIG.

One side of the outer tube 300 is seated on the upper side of the base frame 200 and the other side is extended to the outside of the base frame 200. Both ends of the outer tube 300 are installed on both sides of the upper end of the table 900 And is supported by a support portion 910.

At this time, an opening / closing door 911 for opening the outer tube 300 may be installed on one or both of the pair of supporting portions 910, and a vacuum pump (not shown) may be installed on one or both of the supporting portions 910. [ Or a cooler (not shown).

The inner tube 400 is inserted into the outer tube 300. At this time, the inner tube 400 may be formed by connecting a plurality of unit tubes (not shown) continuously in the longitudinal direction. The outer tube 300 and the inner tube 400 are preferably made of quartz or glass.

The cover 500 is provided to open and close the upper side of the base frame 200 and may be hinged to one side of the longitudinal edge of the base frame 200, for example. When the cover 500 is closed, one side of the outer tube 300 is wrapped by the base frame 200 and the cover 500.

A plurality of heaters 600 are provided on the inner side of the base frame 200 and the cover 500. The material to be purified is vaporized by the heat generated by the heater 600. In order to prevent the heat generated from the heater 600 from being transmitted to the surroundings, it is preferable that a heat insulating material is provided inside the base frame 200 and the cover 500.

According to an embodiment of the present invention, the outer tube 300 is elongated to extend through the base frame 200, and therefore, when the heater 600 is heated, the outer tube 300, which corresponds to the base frame 200 and the cover 500, Only one side of the heater 300 is directly heated by the heat generated from the heater 600.

At least one cooling jacket 700 is coupled to the outer circumferential surface of the outer tube 300 along the longitudinal direction at the other side of the outer tube 300 extending to the outside of the base frame 200.

A plurality of cooling jackets 700 may be sequentially coupled to the outer circumferential surface of the outer tube 300 along the longitudinal direction and refrigerant of different temperatures may be supplied to the respective cooling jackets 700, The temperature of the other side can be set to a different temperature for each section.

At this time, a low temperature temperature gradient is formed in the section of the inner tube 400 corresponding to the coupling section of the cooling jacket 700. In the embodiment shown in FIG. 2, three cooling jackets 700 are coupled, The specifications such as the number and length of the cooling jacket 700 can be appropriately selected as needed.

The cooling jacket 700 according to an embodiment of the present invention includes a hollow body 720 (see FIG. 4) having a hollow portion 721 (see FIG. 4) formed along the periphery of the hollow portion 710 Can be formed in the form of a tube. At this time, both ends of the space portion 721 of the body 720 are closed, and one side and the other side in the longitudinal direction of the body 720 are connected to a refrigerant inlet port 722 (see FIG. 4) communicating with the space portion 721, 723, see Fig. 4).

The cooling jacket 700 in the form of a hollow tube is inserted into the outer circumferential surface of the outer tube 300 and is made of a transparent material such as quartz, glass or plastic so as to check the state of the sample to be solidified on the inner circumferential surface of the inner tube 400 .

The coolant supply device 800 is provided at one side of the base frame 200 for supplying coolant to the cooling jacket 700 and includes a coolant supply pump 810 and a supply pipe 820 and a discharge pipe 830 .

The coolant supply pump 810 may be installed at a lower portion of the base frame 200 as shown in FIG. 2, for example, and the supply pipe 820 may be connected to the coolant supply pump 810 and the coolant inlet And the discharge pipe 830 connects the refrigerant supply pump 810 and the refrigerant discharge port 723 of the cooling jacket 700. [

The refrigerant introduced into the cooling jacket 700 along the supply pipe 820 by the coolant supply pump 810 is cooled by the coolant supply pump 810 along the discharge pipe 830 after cooling the outer tube 300 Is recovered.

The refrigerant may be stored in a storage tank (not shown) provided in the refrigerant supply pump 810 or in a storage tank prepared separately from the refrigerant supply pump 810 .

In addition, in the case where a sample to be solidified on the inner circumferential surface of the inner tube 400 is affected by light through a transparent cooling jacket 700, it is preferable to add a dye having a hue to the refrigerant so as to block light .

At this time, a heat insulating coating layer (not shown) for preventing condensation may be formed on the inner circumferential surface of the cooling jacket 700. This heat insulating coating layer may also have an effect of blocking light.

The temperature of the cooling jacket 700 can be controlled to be constant by controlling the flow rate of the coolant supplied to the cooling jacket 700. A heat exchanger such as a heater or a cooler , The temperature of the supplied refrigerant itself can be controlled.

The plurality of cooling jackets 700 may be connected to the plurality of cooling jackets 700 through a plurality of coolant supply pumps 810. The coolant jackets 700 may be connected to the cooling jackets 700 of the outer tubes 300 at different temperatures So that a gradient is formed.

Meanwhile, as another embodiment of the present invention, the cooling jacket 700 may include a metal case (not shown) and a cooling line (not shown) provided inside the case.

The case may be formed in the same shape as the base frame 200 and the cover 500 described above or in a form in which the base frame 200 and the cover 500 are integrated with each other. (820) and a discharge pipe (830) for discharging the refrigerant.

At this time, a viewport window (not shown) made of a transparent material is preferably provided on one side of the outer circumferential surface of the case so that the state of the sample to be solidified on the inner circumferential surface of the inner tube 400 can be confirmed.

In addition, the cooling line may be provided in various forms such as a horizontal type, a vertical type, a circular type, or a spiral type in the inside of the case, and on the inner side of the cooling jacket 700 and the cooling line, An insulating coating layer may be formed.

FIG. 3 is a cross-sectional view of a cooling jacket according to an embodiment of the present invention, and FIG. 4 is a longitudinal sectional view of a cooling jacket according to an embodiment of the present invention.

3 and 4, the cooling jacket 700 according to an embodiment of the present invention is in the form of a hollow tube coupled to the outer circumferential surface of the outer tube 300. Inside the outer tube 300, (400) is seated.

A space 721 is formed in the body 720 to surround the hollow 710 of the cooling jacket 700 and a coolant is supplied to the body 720. One side of the body 720 in the longitudinal direction and the other side A refrigerant inlet port 722 and a refrigerant outlet port 723 are formed on the outer circumferential surface to communicate with the space portion 721, respectively.

Meanwhile, the cooling jacket 700 according to the above-described embodiment has a function of cooling the outer tube 300 by supplying coolant, and a cooling line is installed inside a case of a block type in which the outer tube 300 penetrates And may be designed in various forms according to the cooling method.

FIG. 4 is a schematic view showing a vaporizing unit and an obtaining unit according to an embodiment of the present invention.

A section corresponding to the base frame 200 and the cover 500 provided with the heater 600 is a vaporizing section A in which the material to be purified sublimates and a section in which the cooling jacket 700 is coupled is composed of a refining material and impurities (B) which solidifies.

At this time, the acquisition section B includes a first low-temperature cooling section B1 to which the first cooling jacket 701 is coupled, a second low-temperature cooling section B2 to which the second cooling jacket 702 is coupled, And the third low-temperature cooling section B3 to which the cooling jacket 703 is coupled. By controlling the temperature of the coolant supplied to each of the cooling jackets 701, 702, 703, Can be set differently from each other.

For example, the temperature of the vaporizing portion A can be set to 50 占 폚 under the control of the heater 600, and the temperature of the refrigerant supplied to each of the low temperature cooling portions B1, B2, The temperature of the cooling section B1 is set to 0 ° C to 20 ° C, the temperature of the second low temperature cooling section B2 to -10 ° C to 0 ° C and the temperature of the third low temperature cooling section B3 to -20 ° C to -10 ° C (The exemplified temperature range is only an example, and the temperature range can be appropriately adjusted depending on the type of material and purpose).

In this case, the material sublimated in the vaporizing portion A concentrates the refining material in any one of the first to third low-temperature cooling portions B1, B2, and B3 (for example, B2) (For example, B1 and B3) are coagulated.

That is, according to one embodiment of the present invention, by forcibly lowering the temperature of the acquisition section B by the cooling jacket 700, even in the case of a material having a low sublimation temperature, The crystallization temperature required for solidification can be set low.

The cooling jacket 700 according to an embodiment of the present invention may be installed at both ends of the outer tube 300. The cooling jacket 700 may be installed in the support portion 910 to prevent impurities from entering the vacuum pump and preventing heat transfer. It is possible to eliminate the cooler provided in the conventional support portion 910, thereby reducing the facility cost.

A:
B: Acquisition unit
100: Low temperature sublimation purification apparatus
200: base frame
300: outer tube
400: inner tube
500: cover
600: heater
700: Cooling jacket
800: Refrigerant supply device
900: Table

Claims (11)

A base frame;
An outer tube having one side seated on the upper side of the base frame;
An inner tube inserted into the outer tube;
A cover coupled to an upper portion of the base frame; And
And a heater disposed inside the base frame or the cover,
Wherein at least one cooling jacket is coupled to the other side of the outer tube extending outside the base frame.
The method according to claim 1,
Wherein a plurality of cooling jackets are coupled to the other side of the outer tube so that a low temperature temperature gradient is formed inside the inner tube extending outside the base frame.
The method of claim 2,
Wherein at least one of the plurality of cooling jackets is supplied with a refrigerant at a different temperature.
The cooling jacket according to claim 1,
And a hollow tube coupled to an outer circumferential surface of the outer tube so as to surround the outer tube.
The cooling jacket according to claim 4,
Wherein the sample is made of a transparent material so that the state of the sample to be obtained can be confirmed.
The method according to claim 1,
And a coolant supply device is provided on one side of the base frame to supply the coolant to the cooling jacket.
The method according to claim 1,
Wherein the cooling jacket is made of a transparent material, and a color dye is added to the refrigerant supplied to the cooling jacket for blocking light.
The refrigerating machine of claim 6,
A supply pipe connected to supply the coolant to the cooling jacket from the coolant supply pump, and a discharge pipe connected to discharge the coolant from the coolant jacket to the coolant supply pump, Temperature sublimation purification apparatus.
The cooling jacket according to claim 1,
A case made of a metal to be coupled to surround the outer tube; and at least one cooling line provided inside the case.
The method of claim 9,
Wherein a viewport window is provided on one side of the case so as to confirm the state of the sample to be taken.
The method according to claim 1,
And a heat insulating coating layer is formed on an inner surface of the cooling jacket.

Images