JP5946252B2 - Purification equipment - Google Patents

Description

  The present invention relates to a technical field of a purification apparatus, and more particularly to a purification apparatus capable of obtaining a high-purity substance.

At present, an organic light emitting diode (OLED: organic EL) is formed by laminating thin films of an organic material, and the organic material for forming the organic thin film is manufactured by a chemical synthesis method.
However, since the reaction of chemical synthesis is performed in a solvent, even if the solvent is removed by heating, the solvent is mixed as an impurity in the organic material obtained by the chemical reaction.

Further, the chemical synthesis reaction does not always proceed according to the theoretical formula, and there is a problem that a chemical substance other than the target chemical substance is also synthesized in a very small amount.
When such an organic material is made into a thin film, the light emission performance and the lifetime are deteriorated due to the mixed impurities.
Therefore, the organic material obtained by chemical synthesis needs to be purified and used once in a vacuum.

FIG. 3 shows a purification apparatus 101 used for the purification, and the purification apparatus 101 has a heating chamber 150.
The heating chamber 150 has an elongated shape, and is configured such that a gas introduction device 123 is connected to one end and a carrier gas is supplied from the gas introduction device 123 to the connection portion, and the other end is connected to the vacuum exhaust device 170. When the evacuation apparatus 170 is connected and operated, the inside of the heating chamber 150 can be evacuated.

In the heating chamber 150, the vaporization container 115, the condenser 152, and the impurity recovery device 159 are arranged in this order from the position of the portion connected to the gas introduction device 123.
When the carrier gas is introduced by the gas introduction device 123 while the inside of the heating chamber 150 is evacuated by the evacuation device 170, the introduced carrier gas moves to the position where the vaporization container 115, the condenser 152, and the impurity recovery device 159 are arranged. It flows in that order and is evacuated.

A high temperature heating device 154 is provided on the outer periphery of the portion of the heating chamber 150 where the vaporization vessel 115 is located, and low temperature heating is provided on the outer periphery of the portion where the condenser 152 is located and the portion where the impurity recovery device 159 is located. A device 155 is provided.
The high temperature heating device 154 and the low temperature heating device 155 are each connected to a power source, and when a voltage is applied from the power source, the high temperature heating device 154 is heated to a higher temperature than the low temperature heating device 155.

Inside the vaporization vessel 115, a purification object that is refined to improve the purity is disposed, and the purification object is heated by the heat generated by the high-temperature heating device 154 to a temperature equal to or higher than the vaporization temperature (including the sublimation temperature). The temperature is raised and a gas to be purified is generated.
The produced gas to be purified is transported by the carrier gas and moves to the position where the condenser 152 is disposed.

  The condenser 152 is heated to a temperature higher than room temperature and lower than the sublimation temperature of the object to be purified by the low-temperature heating device 155, and when the gas of the object to be purified comes into contact with the condenser 152, Gas is deposited on the condenser 152.

  The evaporation temperature of the residual solvent mixed in the object to be purified is lower than the temperature at which the object to be purified sublimates, but the temperature of the condenser 152 is set higher than the evaporation temperature of the residual solvent. This gas is not condensed in the condenser 152.

  An impurity recovery device 159 having a temperature lower than the evaporation temperature of the residual solvent is arranged in the traveling direction of the gas of the purification object that has passed through the condenser 152, and the residual solvent gas mixed in the gas of the purification object Contact with each other, the object to be purified and the residual solvent condense inside the condenser 152 (including solid precipitation).

After the purification object in the vaporization vessel 115 is completely vaporized and the purification object is deposited on the condenser 152, the heat generation by the high temperature heating device 154 and the low temperature heating device 155 is terminated, and the condenser 152 is lowered to a predetermined temperature. After that, the evacuation of the heating chamber 150 and the supply of the carrier gas are stopped, the purge gas is supplied from the purge gas supply device 158 into the heating chamber 150, and the pressure is changed to the atmospheric pressure. The condenser 152 is removed from the heating chamber 150.
A purification object is disposed in the vaporization vessel 115, and a condenser 152 to which the purification object is not attached is disposed in the heating chamber 150, and the purification of the purification object is resumed.

JP 2003-095992 A JP-A-2005-161251 JP 2007-044592 A

However, the purification apparatus 101 requires a long cooling time and reheating time when the condenser 152 is taken out of the heating chamber, and the use efficiency of the apparatus is poor.
In addition, in order to obtain a large amount of a purification object by a single take-out operation, if the condenser 152 is placed in the heating chamber 150 for a long time to deposit the gas of the purification object, the precipitated purification The part heated for a long time among the objects will deteriorate. Moreover, when it precipitates in large quantities, the temperature of the condensation part of the condenser 152 will change, and purity will fall.
Furthermore, in the conventional purification apparatus 101, it is difficult to improve the purity of the purified purification target, and it is desired to realize a purification apparatus that solves these problems.

In order to solve the above-described problems, the present invention is configured to be evacuated and to which a purification target is placed, and the purification target is supplied from the supply chamber, and the purification target is placed in a vacuum atmosphere. When the inlet valve is opened while one end on the inlet side is connected to the vaporizer chamber via an introduction valve and one end on the outlet side is evacuated, the vaporization chamber is heated to generate the gas to be purified. A product gas, which is a gas generated in a room, is introduced into the interior, and the product gas is configured to flow from one end on the inlet side toward one end on the outlet side, and is arranged in parallel. A condensing chamber, a plurality of condensers arranged in the condensing chamber and arranged side by side between the inlet side one end and the outlet side one end, and a condenser provided in the condensing chamber and close to the inlet side one end A higher temperature than the far condenser A heating device for heating, and a shutoff valve is provided between the supply chamber and the vaporization chamber, and the internal atmosphere of the supply chamber and the vaporization chamber is connected when the shutoff valve is opened, A purification device to be separated when closed , wherein the supply chamber is provided with a funnel-shaped supply container, and a funnel-shaped lower tubular portion of the supply container is inserted into the vaporization chamber, The rotary shaft having a screw groove around it is inserted, and the powdery purification object placed in the supply container is rotated from the supply chamber to the vaporization chamber by the rotation of the rotary shaft. It is a purification device to which an object is moved .
Also, the present invention is, in the inlet side, wherein the condenser is heated to a temperature higher than the vaporization or sublimation temperature of the purified target is a plurality of arranged, wherein on the outlet side, the purified target vaporization Alternatively, a plurality of the condensers that are heated to a temperature lower than the sublimation temperature are arranged, and between the condenser having a temperature higher than the temperature at which the purification target is vaporized or sublimated and the condenser having a lower temperature. Is a purification apparatus in which a plurality of the condensers are arranged.

According to the present invention, since a large amount of the purification object arranged in the supply container can be generated using a plurality of condensing chambers, purification can be performed by another condensing chamber even while one condensing chamber is cooled. Therefore, it is not necessary to stop the generation of the gas to be purified.
By making the inside of the supply chamber a vacuum atmosphere, it is possible to prevent moisture from adhering to the purification object.
In addition, the temperature can be raised to a temperature at which moisture does not adhere to the purification target in a vacuum atmosphere.

In one condensing chamber, the precipitation of the purification object is terminated, and while the cooling object is cooled, taken out, evacuated, and the condenser is reheated, the purification object is precipitated in the other condensing chamber. Even if the object to be purified is placed in the supply container, the precipitation is not interrupted.
Further, if a plurality of condensers are arranged in the condensing chamber so that the temperature of the condenser can be set finely, the purity of the purification object to be obtained can be increased.

  The purification object in the supply container is not heated to a high temperature, and only a small amount of the purification object is supplied to the vaporization chamber, so that the time for which the purification object is heated is short and the purification object deposited in the condensation chamber Since the object is not heated for a long time, the object to be purified does not deteriorate.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. Drawing for explaining the condenser Drawing for explaining a conventional purification apparatus

Reference numeral 1 in FIG. 1 represents an example of the purification apparatus of the present invention.
The purification device 1 includes a gas generation device 3 and a condensate generation device 5, and a purification target 16 made of an organic compound synthesized in the gas generation device 3 is arranged to generate a gas of the purification target 16. If it is made to supply to the condensate production | generation apparatus 5, gas will be made into solid by the condensate production | generation apparatus 5. FIG.

  In the condensate production | generation apparatus 5, it is comprised so that a purity may differ in a different position, and when a high purity condensate is collected by excluding a low purity condensate, vaporization (this invention In this case, a purified product having a purity higher than that of the purified object 16 to be sublimated) is obtained.

  First, the gas generation device 3 will be described. The gas generation device 3 includes a supply chamber 10 in which a large amount of the purification object 16 is disposed and a vaporization chamber 20 in which the purification object 16 is supplied in small amounts from the supply chamber 10. Have. The supply chamber 10 and the vaporization chamber 20 are vacuum tanks and can be evacuated. A shutoff valve 31 is provided between the supply chamber 10 and the vaporization chamber 20, and the interior is connected when the shutoff valve 31 is opened, and the internal atmosphere of the supply chamber 10 and the vaporization chamber 20 is separated when the shutoff valve 31 is closed. It has become so.

The supply chamber 10 is provided with a funnel-shaped supply container 15.
The vaporization chamber 20 is disposed below the supply chamber 10, and the tubular portion 22, which is the lower end of the funnel shape of the supply container 15, is inserted into the vaporization chamber 20.

  The inside of the vaporizing chamber 20 and the inside of the supply chamber 10 are cut off from the outside, and the inside of the vaporizing chamber 20 and the inside of the supply chamber 10 are connected by a funnel lower end portion of the supply container 15 in a state where a vacuum atmosphere can be formed. ing.

A rotating shaft 13 having a spiral thread groove 14 formed on the side surface is inserted into the tubular portion 22. The lower tubular portion of the supply container 15 is closed by the rotating shaft 13, and the powder does not fall through the tubular portion below the funnel.
In this example, the purification object 16 is a powdered organic compound, and the purification object 16 is arranged in the supply container 15 with the rotating shaft 13 inserted.

  In the lower tubular portion of the supply container 15, the powder purification object 16 is filled in the groove on the side surface of the rotating shaft 13. It passes through the tubular portion 22 and falls into the vaporizing chamber 20.

The purification object 16 drops by an amount corresponding to the rotation amount of the rotary shaft 13, and the purification object 16 falls from the supply chamber 10 to the vaporization chamber 20, whereby the purification object 16 is supplied from the supply chamber 10 to the vaporization chamber 20. 16 is supplied.
A container-like heating container 21 is provided inside the vaporization chamber 20, and the purification target 16 that falls into the vaporization chamber 20 is supplied to the heating container 21.

  When the inside of the vaporizing chamber 20 is evacuated, the inside of the heating vessel 21 is also evacuated, and the purification object 16 supplied is supplied in a state where the inside of the supply vessel 15 and the inside of the vaporizing chamber 20 are in a vacuum atmosphere. However, when heated by the vaporization heating device 24 provided in the vaporization chamber 20, the purification object 16 changes from a solid powder state to a gas state inside the heating container 21, and the heating container 21 is filled. To do.

  If the purification target 16 disposed in the supply chamber 10 is contaminated with impurities and the gas generated in the vaporization chamber 20 is a generated gas, the generated gas is an impurity in the gas of the purification target. This gas is a mixture of gases.

  In this example, an evacuation device 7 is connected to the supply chamber 10, and the evacuation device 7 operates to evacuate the interior of the supply chamber 10 to a vacuum atmosphere. Moisture does not adhere to the object 16. Further, the temperature can be raised to a temperature at which moisture does not adhere to the purification object 16 in a vacuum atmosphere.

  The inside of the vaporizing chamber 20 is evacuated by the vacuum evacuation device 7 through the supply chamber 10, and the inside of the heating vessel 21 is evacuated through the supply vessel 15. By the rotation of the rotating shaft 13, a small amount of the purification object is continuously supplied from the supply container 15 to the heating container 21 so as to reach a constant supply speed. The gas of the purification target 16 is continuously generated by being heated by the heating device 24.

  Next, the condensate generator 5 will be described. The condensate generator 5 has a plurality of condensing chambers 50a and 50b (two in this case). Each of the condensing chambers 50 a and 50 b has an elongated cylindrical body 53, and an inlet valve 51 is provided at one end 11 on the inlet side of the cylindrical body 53. The heating vessel 21 in the vaporization chamber 20 and the introduction valves 51 of the condensing chambers 50a and 50b are connected to each other by a branched pipe 41. When the introduction valve 51 is opened, the introduction valve 51 is opened. The inside of the cylindrical body 53 of the condensation chambers 50a and 50b brought into the state is connected to the inside of the heating container 21.

The vacuum exhaust device 7 is connected to the outlet side one end 12 of the cylinder 53 of each condensing chamber 50a, 50b via a cooling device 56. The condensation chambers 50a and 50b are formed in an airtight manner, and the inside of the cylinder 53 is configured to be evacuated when the evacuation device 7 is operated with the introduction valve 51 closed. Here, each of the condensing chambers 50a and 50b is evacuated, and the inside of the cylinder 53 is in a vacuum atmosphere at a predetermined pressure or lower.
The condensation chambers 50a and 50b and the supply chamber 10 may be evacuated by the same evacuation device 7 or evacuated by different evacuation devices.

  A carrier gas supply device 23 is connected to the heating container 21, and a supply valve 25 is provided in a pipe 26 that connects the heating container 21 and the carrier gas supply device 23.

  The inlet valve 51 of each condensing chamber 50a, 50b is closed, and the supply valve 25 is opened while the inside of the cylinder 53 of each condensing chamber 50a, 50b is evacuated by the evacuation device 7, and the heating container 21 and carrier gas are supplied. The device 23 is connected.

  Next, when the introduction valve 51 of the desired condensation chamber (here, 50a) is changed from the closed state to the opened state, and the purification target 16 is supplied from the supply chamber 10 into the vaporization chamber 20, the inside of the vaporization chamber 20 and the condensation chamber are supplied. Due to the pressure difference in the cylinder 53 of 50a, the generated gas generated in the vaporization chamber 20 moves together with the carrier gas into the cylinder 53 of the condensation chamber 50a in which the introduction valve 51 is opened.

In this example, the generated gas and the carrier gas introduced into the cylinder 53 of the condensing chamber 50 a flow through the cylinder 53 and are evacuated through the cooling device 56.
Inside the cylindrical body 53 of the condensing chamber 50 a, a condenser 52 in contact with the generated gas is arranged side by side between the inlet side one end 11 and the outlet side one end 12. Here, they are arranged in a line along the flow of the product gas and the carrier gas.

  A heating device 54 is provided on the wall surface of the cylindrical body 53 along the longitudinal direction of the cylindrical body 53, and the wall of the cylindrical body 53 and each condenser 52 disposed in the cylindrical body 53 are connected to the heating device 54. It is supposed to be heated by. The heating device 54 heats the condenser 52 in the cylindrical body 53 to a high temperature at the condenser 52 at a position close to the introduction valve 51, and heats the condenser 52 at a position farther than that to a lower temperature than a near position.

Therefore, the condenser 52 arranged side by side in the longitudinal direction in the cylindrical body 53 has a lower temperature from the upstream side to the downstream side of the gas flowing inside.
On the upstream side, the plurality of condensers 52 are heated to a temperature higher than the vaporization temperature of the purification object 16 (sublimation temperature for sublimated solids), and on the downstream side, the plurality of condensers 52 are to be purified. It is heated to a temperature lower than the vaporization temperature of the object 16.

  A plurality of condensers 52 are arranged between the condenser 52 having a temperature higher than the vaporization temperature of the purification object 16 and the condenser 52 having a low temperature, and the temperature is higher than the vaporization temperature of the purification object 16. A plurality of condensers 52 and a plurality of low-temperature condensers 52 are arranged.

The impurities mixed in the purification target object 16 include a high temperature impurity that vaporizes at a temperature higher than the temperature at which the purification target object 16 vaporizes and a low temperature impurity that vaporizes at a low temperature.
The product gas introduced into the cylindrical body 53 of the condensing chamber 50a includes a high-temperature impurity gas and a low-temperature impurity gas in addition to the gas of the purification target 16.
Furthermore, the high temperature impurity and the low temperature impurity are each composed of a plurality of substances, and have different vaporization temperatures or sublimation temperatures for each substance.

  When the product gas and the carrier gas introduced into the vaporization chamber 20 first contact with the high-temperature condenser 52 on the inlet side, the high-temperature chemical substance whose vaporization temperature is higher than the temperature of the condenser 52 in contact is condensed. (Or solidifies), and the high-temperature impurity gas is removed or reduced from the generated gas flowing in the cylinder 53.

As shown in FIG. 2, each condenser 52 has a ring shape, and the gas flowing in the cylindrical body 53 flows through the inside of each condenser 52 so that the condensate grows on the inner peripheral surface. It has become.
If the condenser 52 arranged at the top is the highest temperature, the condenser 52 of the second temperature arranged next to the condenser 52 is the second highest temperature, and the product that has passed through the condenser 52 at the top is generated. When the gas contacts the second condenser 52, the high-temperature impurity gas having a higher vaporization temperature than the second temperature is condensed into a solid or liquid.

  In this way, the product gas introduced into the cylinder 53 of the condensation chamber 50 a is heated from the high-temperature condenser 52 to the low-temperature condenser 52 by the condenser 52 heated to a temperature equal to or higher than the vaporization temperature of the purification target 16. When the contact is made in order, the high-temperature impurities having a vaporization temperature corresponding to the temperature of each condenser 52 are condensed (including the case where a solid is precipitated in the present invention), and the high-temperature impurities are removed from the product gas.

  Thereafter, when the product gas from which the high temperature impurities have been removed contacts the condenser 52 having a temperature lower than the vaporization temperature of the purification target object 16, the purification target object 16 is condensed and the purification target object 16 is deposited on the condenser 52. .

  The gas of the purification target 16 is contained in a large amount in the product gas introduced into the vaporization chamber 20, and is condensed by the leading condenser 52 among the condensers 52 having a temperature lower than the vaporization temperature of the purification target 16. A large amount is also contained in the gas that has passed without being purified, and even in the condenser 52 having a temperature lower than the vaporization temperature of the object 16 to be purified, the condenser 52 having the second highest temperature after the leading condenser 52 is also purified. The object 16 is condensed.

  Further, the purification object 16 is condensed in the condenser 52 having the next highest temperature. Thus, the purification object 16 is condensed in the condenser 52 having a temperature lower than the vaporization temperature of the purification object 16.

In the present embodiment, the temperature of the condenser 52 is lowered in the order arranged from the upstream side toward the downstream side, and impurities having a low vaporization temperature are easily solidified in the condenser 52 having a low temperature. In the condenser 52 having a temperature lower than the vaporization temperature of the object 16 to be purified, the content of impurities increases in the condenser 52 having a temperature lower than a predetermined minimum temperature.
Therefore, in the condenser 52 having a temperature lower than the vaporization temperature of the purification object 16, the condensate of the condenser 52 having a temperature equal to or higher than the minimum temperature is the high-purity purification object 16.

  The product gas and the carrier gas that are not condensed in each condenser 52 flow through the cylindrical body 53 and enter the inside of the cooling device 56. A cooling device 56 that is cooled to a temperature lower than room temperature is disposed inside the cooling device 56, the generated gas that has contacted the cooling device 56 is condensed, and the carrier gas passes through the inside of the vacuum exhaust device 7. It is evacuated.

When the product gas condensate introduced into each condenser 52 grows, the introduction valve 51 is closed, the heating device 54 is stopped, and the condensate is cooled.
When the condensate is cooled to a predetermined temperature or lower, the evacuation of the condensation chamber 50a is stopped, purge gas is introduced from the purge gas supply device 58 into the cylinder 53 of the condensation chamber 50a, and the cylinder 53 is condensed to atmospheric pressure. The door (not shown) of the cylinder 53 of the chamber 50a is opened, and the condenser 52 to which the condensate is attached is taken out.

  Of the condenser 52 taken out, the purity of the deposits of the condenser 52 that has been heated to a predetermined temperature range is high. Is obtained.

  In this embodiment, among the plurality of condensation chambers 50a and 50b evacuated, the introduction valves 51 of one or more condensation chambers 50a are opened, and the introduction valves 51 of the other one or more condensation chambers 50b are closed. When the product gas is supplied from the vaporizing chamber 20 to the condensing chamber 50a in which the introducing valve 51 is opened and a predetermined amount of condensate grows in the condenser 52, the introducing valve 51 in the condensing chamber 50a is closed and condensed. When entering the state of cooling the product, the introduction valve 51 of the condensing chamber 50b in which the condenser 52 to which no condensate is attached is opened, and the growth of the condensate in the condensing chamber 50b is started.

  On the other hand, in the condensing chamber 50a from which the condenser 52 has been taken out, the condenser 52 to which no condensate is attached is disposed at a predetermined position, and after the door is closed and shut off from the atmosphere, the vacuum exhaust inside the condensing chamber 50a is removed. Be started.

  As described above, in the present invention, the plurality of condensing chambers 50a and 50b are connected in parallel to the same gas generator 3. In one or a plurality of condensing chambers 50a, the introduction valve 51 is closed to cool and condense the condenser 52. Or in the middle of the vacuum evacuation to a predetermined pressure, during which time the condensation object can be condensed in the condenser 52 in the other condensation chamber 50b.

  In short, in the present invention, a large amount of the purification object 16 arranged in the supply container 15 is vaporized in one vaporizing chamber 20 to generate a generated gas, and the generated gas is condensed in a plurality of condensing chambers 50a and 50b. At this time, since the condensate can be obtained by opening the introduction valve 51 at different times to start the condensation, it is not necessary to stop the condensation during the cooling time or the evacuation time.

  In addition, when a small amount of condensate adheres, condensation can be stopped and condensation can be started in the other condensing chamber 50b during cooling, thus preventing temperature changes caused by attaching a large amount of condensate. And a decrease in purity can be suppressed.

  Further, among the condensers 52 that are lower than the vaporization temperature of the purification object 16 and heated to a temperature that is equal to or higher than the minimum temperature, the condenser 52 having a high temperature has a high purity and a low temperature. The purity of the 52 condensate is low.

  The deposit on the condenser 52 heated to a temperature higher than the vaporization temperature of the purification object 16 is discarded, but the condensate in the condenser 52 lower than the minimum temperature is vaporized again to condense chambers 50a and 50b. If it is introduced into the inside and condensed, a highly pure condensate can be obtained, and even the condenser 52 heated to a temperature higher than the minimum temperature is condensed at a relatively low temperature, and the condensate having a low purity. However, even these low-purity condensates are higher in purity than the purification target 16 that has not been vaporized / condensed, so these condensates are collected, vaporized again, and introduced into the condensation chambers 50a and 50b for condensation. If so, it is easy to obtain a high-purity condensate.

  In the present invention, when the condensate is grown in one or a plurality of condensing chambers 50a and 50b and the purification target 16 disposed in the supply container 15 is lost, the condensate obtained is obtained. While the introduction valve 51 of the chambers 50a and 50b is closed and the condenser 52 in the condensation chambers 50a and 50b is cooled, the purification object 16 can be arranged in the supply chamber 10.

  Here, a shutoff valve 31 is provided between the supply chamber 10 and the vaporization chamber 20, the lower part of the supply container 15 is extracted from the vaporization chamber 20, and the shutoff valve 31 is provided between the supply chamber 10 and the vaporization chamber 20. Is closed and separated, the exhaust valve between the supply chamber 10 and the vacuum evacuation device 7 is closed, the vacuum exhaust in the supply chamber 10 is stopped, the atmosphere is introduced, and the door of the supply chamber 10 is opened to be purified. The object 16 can be placed in the supply chamber 10.

After the purification object 16 is arranged and the exhaust valve is opened and the supply chamber 10 is evacuated, the shutoff valve 31 is opened and the lower part of the supply container 15 can be inserted into the vaporization chamber 20.
At this time, in the supply chamber 10, a substance different from the condensate of the condenser 52 being cooled is disposed as the purification target 16, and the purification target 16 is supplied to the heating container 21 of the vaporization chamber 20 to be different. The condensates of different substances can be generated in the condensation chambers 50a and 50b by opening the introduction valve 51 of the condensation chambers 50a and 50b in which no condensate is formed.

  In the above embodiment, the generated gas is transported into the cylinder 53 by the carrier gas introduced into the heating container 21, but the generated gas is vaporized by the pressure of the generated gas generated in the vaporizing chamber 20. 20 can be moved into the cylinder 53.

DESCRIPTION OF SYMBOLS 10 ... Supply chamber 11 ... Inlet side one end 12 ... Outlet side one end 13 ... Rotary shaft 15 ... Supply container 16 ... Purification object 20 ... Vaporization chamber 50a, 50b ... Condensing chamber 51 ... Introduction valve 52 …… Condenser

Claims (2)

A supply chamber configured to be evacuated and in which a purification object is disposed;
The purification object is supplied from the supply chamber, a vaporization chamber for heating the purification object in a vacuum atmosphere and generating a gas of the purification object;
One end of the inlet side is connected to the vaporization chamber via an introduction valve, and when the introduction valve is opened while the one end of the outlet side is evacuated, a generated gas, which is a gas generated in the vaporization chamber, is introduced inside, The product gas is configured to flow from one end on the inlet side toward one end on the outlet side, and a plurality of elongated condensation chambers arranged in parallel;
A plurality of condensers arranged in the condensation chamber and arranged side by side between the one end on the inlet side and the one end on the outlet side;
A heating device that is provided in the condensation chamber and that heats the condenser close to the one end on the inlet side to a higher temperature than a far condenser;
Have
The shut-off valve is provided between the supply chamber and said vaporization chamber is provided, the internal atmosphere of the vaporizing chamber and the supply chamber is connected to the shut-off valve is opened, when closed, the purification device to be separated There,
The supply chamber is provided with a funnel-shaped supply container, and the funnel-shaped lower tubular portion of the supply container is inserted into the vaporization chamber,
The tubular portion is inserted with a rotating shaft having a thread groove around it, and the powdery purification target disposed in the supply container is vaporized from the supply chamber by the rotation of the rotating shaft. A purification apparatus in which the object to be purified is moved to a chamber . On the inlet side, a plurality of the condensers that are heated to a temperature higher than the temperature at which the object to be purified is vaporized or sublimated are arranged,
On the outlet side, a plurality of the condensers that are heated to a temperature lower than the temperature at which the purification object is vaporized or sublimated are arranged,
Wherein the purified object the condenser temperature higher than the vaporization or sublimation temperature, between the said condenser low temperature, a plurality of the condenser disposed claims 1 Symbol placement refiner.

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