JP2014061464A - Apparatus and method for sublimation purification - Google Patents

Apparatus and method for sublimation purification Download PDF

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JP2014061464A
JP2014061464A JP2012206616A JP2012206616A JP2014061464A JP 2014061464 A JP2014061464 A JP 2014061464A JP 2012206616 A JP2012206616 A JP 2012206616A JP 2012206616 A JP2012206616 A JP 2012206616A JP 2014061464 A JP2014061464 A JP 2014061464A
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sublimation purification
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heating container
tube
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Kazuhiro Niwa
和裕 丹羽
Shinji Yoshida
真司 吉田
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Panasonic Corp
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Panasonic Corp
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Abstract

PROBLEM TO BE SOLVED: To prevent formation of impurities by heating uniformly and efficiently a substance to be treated so as to improve the purity and yield of the substance sublimation-purified.SOLUTION: A substance 8 to be treated (target substance 8) is charged in a target substance heating container 7 within a sublimation purification tube 2. Inside the sublimation purification tube 2 with the pressure reduced by pressure reducing means 3, the target substance 8 is sublimated by heating the target substance heating container 7. Since the sublimated target substance 8 diffuses within the sublimation purification tube 2, the ingredient condensed on the surface of the inside wall can be recovered as a sublimation-purified substance 12. When an oscillation shaft 9 is twisted right and left under the action of oscillating means 10, the target substance heating container 7 is oscillated with its bottom surface kept in tight contact with the surface of the inside wall of the sublimation purification tube 2, the surface layer of the target substance 8 can be exchanged with its bottom layer, thereby leading to uniform heating of the target substance 8.

Description

本発明は、昇華性を有する有機化合物などを被処理物質として含有する混合物から昇華温度の違いを利用して、被処理物質を精製、分離する昇華精製装置および昇華精製方法に関するものである。   The present invention relates to a sublimation purification apparatus and a sublimation purification method for purifying and separating a substance to be treated using a difference in sublimation temperature from a mixture containing a sublimable organic compound as a substance to be treated.

従来の昇華精製装置および昇華精製方法として、有機化合物の粉末を昇華した後に昇華精製管の内部で凝結させることで昇華精製を行う昇華精製装置が知られている（例えば特許文献１参照）。   As a conventional sublimation purification apparatus and sublimation purification method, there is known a sublimation purification apparatus that performs sublimation purification by sublimating an organic compound powder and condensing inside a sublimation purification tube (see, for example, Patent Document 1).

以下、その昇華精製装置について図７および図８を参照しながら説明する。   Hereinafter, the sublimation purification apparatus will be described with reference to FIGS.

図７に示すように、昇華精製装置１０１は昇華精製管１０２と減圧手段１０３と加熱手段１０４ａ、加熱手段１０４ｂ、加熱手段１０４ｃとフランジ１０５ａ、フランジ１０５ｂからなる。昇華精製管１０２は長手方向の両端に開口部を有する円筒状の形状をしており、加熱手段１０４ａ、加熱手段１０４ｂ、加熱手段１０４ｃは中心に開口部を有するドーナツ形状をしており、昇華精製管１０２の外周部を連続的に覆い、昇華精製管１０２に密着するように配置されている。   As shown in FIG. 7, the sublimation purification apparatus 101 includes a sublimation purification tube 102, a decompression means 103, a heating means 104a, a heating means 104b, a heating means 104c, a flange 105a, and a flange 105b. The sublimation purification tube 102 has a cylindrical shape with openings at both ends in the longitudinal direction, and the heating means 104a, heating means 104b, and heating means 104c have a donut shape with an opening at the center. It arrange | positions so that the outer peripheral part of the pipe | tube 102 may be covered continuously and it closely_contact | adheres to the sublimation purification pipe | tube 102. FIG.

昇華精製管１０２の長手方向両端の開口部は、フランジ１０５ａ、フランジ１０５ｂが固定されており、フランジ１０５ｂは流出口１０６を備えている。途中の配管は省略しているが、フランジ１０５ｂの流出口１０６は減圧手段１０３と接続されている。昇華精製管１０２の内部には被処理物質加熱容器１０７が設置され、被処理物質加熱容器１０７には被処理物質１０８が充填されている。   A flange 105 a and a flange 105 b are fixed to openings at both ends in the longitudinal direction of the sublimation purification pipe 102, and the flange 105 b includes an outlet 106. Although piping in the middle is omitted, the outlet 106 of the flange 105 b is connected to the decompression means 103. A to-be-treated substance heating container 107 is installed inside the sublimation purification tube 102, and the to-be-treated substance heating container 107 is filled with the to-be-treated substance 108.

加熱手段１０４ａ、加熱手段１０４ｂ、加熱手段１０４ｃはそれぞれ電熱線１０９を内蔵している。減圧手段１０３により減圧した昇華精製管１０２の内部において、加熱手段１０４ａの電熱線１０９に通電すると被処理物質加熱容器１０７が加熱されるので被処理物質１０８が昇華する。加熱手段１０４ｃにおいては被処理物質１０８の昇華温度よりもわずかに低い温度で昇華精製管１０２を加熱している。   The heating means 104a, the heating means 104b, and the heating means 104c each include a heating wire 109. In the sublimation purification tube 102 depressurized by the depressurization means 103, when the heating wire 109 of the heating means 104a is energized, the target substance heating container 107 is heated, so that the target substance 108 is sublimated. In the heating means 104c, the sublimation purification tube 102 is heated at a temperature slightly lower than the sublimation temperature of the substance 108 to be treated.

被処理物質加熱容器１０７で昇華された被処理物質１０８は昇華精製管１０２の内部を拡散し、昇華精製管１０２の内壁面の温度が被処理物質１０８の昇華温度すなわち凝結温度よりも低い場所で昇華精製管１０２の内壁面に凝結する。   The to-be-treated substance 108 sublimated in the to-be-treated substance heating container 107 diffuses in the sublimation purification tube 102, and the temperature of the inner wall surface of the sublimation purification tube 102 is lower than the sublimation temperature of the to-be-treated material 108, that is, the condensation temperature. It condenses on the inner wall surface of the sublimation purification tube 102.

この従来の昇華精製装置においては、先に示したように、加熱手段１０４ｃの内側の昇華精製管１０２の内壁面が被処理物質１０８の昇華温度よりも低いので、凝結した成分を昇華精製物質１１０として回収することができる。   In this conventional sublimation purification apparatus, as shown above, since the inner wall surface of the sublimation purification tube 102 inside the heating means 104c is lower than the sublimation temperature of the material 108 to be treated, the condensed components are sublimated and purified 110. Can be recovered.

図８に示すように、被処理物質加熱容器１０７の底面は昇華精製管１０２の内壁面に密着するように湾曲している。また、被処理物質加熱容器１０７の上面は、被処理物質加熱容器１０７を加熱した際に被処理物質１０８が効率良く昇華できるように広い開口部を有している。   As shown in FIG. 8, the bottom surface of the substance heating container 107 is curved so as to be in close contact with the inner wall surface of the sublimation purification tube 102. Further, the upper surface of the target substance heating container 107 has a wide opening so that the target substance 108 can be efficiently sublimated when the target substance heating container 107 is heated.

このような従来の昇華精製装置においては、不純物を含む被処理物質を昇華精製物質として精製するために、減圧下において被処理物質を加熱すると固体から気体へ昇華する特性を利用している。   In such a conventional sublimation purification apparatus, in order to purify a substance to be treated containing impurities as a sublimation purification substance, a characteristic of sublimation from a solid to a gas is used when the substance to be treated is heated under reduced pressure.

つまり、被処理物質と被処理物質に含まれる不純物の昇華温度が異なることから、一定温度で被処理物質を昇華させると、昇華温度の高い不純物は昇華されることがないので、昇華された被処理物質を別の場所で凝結させると、純度の高い昇華精製物質を得ることができる。   In other words, since the sublimation temperature of the impurity to be treated differs from that of the substance to be treated, if the substance to be treated is sublimated at a constant temperature, impurities having a high sublimation temperature are not sublimated. When the treatment substance is condensed at another place, a highly purified sublimation purification substance can be obtained.

また、被処理物質よりも凝結温度の低い不純物は、被処理物質が凝結する場所では凝結しないので、被処理物質が凝結した場所だけから被処理物質を回収することで純度の高い昇華精製物質を得ることができる。   In addition, impurities with a condensation temperature lower than that of the material to be treated do not condense in the place where the material to be treated condenses, so that a highly purified sublimation purification material can be obtained by collecting the material to be treated only from the place where the material to be treated has condensed. Can be obtained.

昇華精製方法は被処理物質に含まれる不純物と被処理物質の昇華温度すなわち凝結温度の違いを利用して、昇華精製管の内壁面に純度の高い昇華精製物質を凝結させる方法であり、被処理物質の昇華温度以上かつ分解温度以下の適正な温度条件で被処理物質を昇華させる必要がある。   The sublimation purification method is a method of condensing a high-purity sublimation purification material on the inner wall surface of a sublimation purification tube by utilizing the difference between the impurities contained in the treatment material and the sublimation temperature of the treatment material, that is, the condensation temperature. It is necessary to sublimate the substance to be treated under an appropriate temperature condition that is higher than the sublimation temperature of the substance and lower than the decomposition temperature.

また、昇華精製管の内壁面の温度は被処理物質の凝結温度以下で安定していることが重要である。したがって、昇華精製中に被処理物質を凝結させる昇華精製管の内壁面の温度を安定させるために、昇華精製管の全周にわたって加熱手段を備える構成となっている。   In addition, it is important that the temperature of the inner wall surface of the sublimation purification tube is stable below the condensation temperature of the material to be treated. Therefore, in order to stabilize the temperature of the inner wall surface of the sublimation purification tube that condenses the substance to be treated during sublimation purification, the heating means is provided over the entire circumference of the sublimation purification tube.

有機半導体や有機色素のように昇華精製方法を適用する被処理物質は、酸素または水分を含む雰囲気下では分解されやすい特性であることが多く、微量の不活性ガスを注入または充填した状態で昇華精製する場合もある。   Substances to be treated, such as organic semiconductors and organic dyes, to which sublimation purification methods are applied are often easily decomposed in an atmosphere containing oxygen or moisture, and are sublimated in a state where a small amount of inert gas is injected or filled. It may be purified.

特開２００７−２４６４２４号公報JP 2007-246424 A

このような従来の昇華精製装置および昇華精製方法においては、昇華精製に要する時間を短縮する目的で、被処理物質加熱容器から昇華する被処理物質を増やすために、被処理物質の加熱温度を上げることがある。   In such a conventional sublimation purification apparatus and sublimation purification method, in order to shorten the time required for sublimation purification, the heating temperature of the material to be treated is increased in order to increase the number of materials to be sublimated from the material to be treated heating container. Sometimes.

しかし、被処理物質が粉末状であること、および、昇華精製管の内部が真空状態であることから、被処理物質加熱容器からの熱伝導により被処理物質を加熱するためには被処理物質内部の熱伝導効率が低く、被処理物質加熱容器と被処理物質の接触部分が先に加熱されてしまう。   However, since the substance to be treated is in the form of powder and the inside of the sublimation purification tube is in a vacuum state, in order to heat the substance to be treated by heat conduction from the substance to be treated heating container, Therefore, the contact portion between the target substance heating container and the target substance is heated first.

その結果、被処理物質加熱容器に充填された被処理物質の表面温度が昇華温度に達する前に、被処理物質加熱容器と被処理物質の接触部分が被処理物質の分解温度を超えてしまい、被処理物質が分解されてしまうことがあった。   As a result, before the surface temperature of the material to be treated filled in the material to be treated reaches the sublimation temperature, the contact portion between the material to be treated and the material to be treated exceeds the decomposition temperature of the material to be treated, The material to be treated might be decomposed.

分解された被処理物質は組成が変わることにより被処理物質とは異なる性状となるが、被処理物質と同様に昇華され、昇華精製管の内壁面に不純物として付着した場合には、昇華精製管から回収する昇華精製物質の純度を低下させる。また、液状の物質に変成した場合には被処理物質加熱容器内で被処理物質に付着して、被処理物質の昇華を妨げることとなり、昇華精製物質の収率を低下させる。   The decomposed material to be treated has a different property from the material to be treated due to the composition change. However, if the material is sublimated in the same manner as the material to be treated and adheres as an impurity to the inner wall surface of the sublimation purification tube, the sublimation purification tube The purity of the sublimation purification material recovered from the product is lowered. Moreover, when it transform | converts into a liquid substance, it will adhere to a to-be-processed substance in a to-be-processed substance heating container, will prevent sublimation of a to-be-processed substance, and will reduce the yield of a sublimation refinement | purification substance.

つまり、従来の昇華精製装置および昇華精製方法は、被処理物質を昇華させる際に、被処理物質が不均一に加熱されることにより昇華精製物質の純度低下や収率低下が発生するという課題を有していた。   In other words, the conventional sublimation purification apparatus and the sublimation purification method have a problem that when the material to be treated is sublimated, the material to be treated is heated non-uniformly, resulting in a decrease in the purity and yield of the sublimation purification material. Had.

そこで本発明は、上記従来の課題を解決するものであり、被処理物質を均一に加熱することにより昇華精製物質の純度および収率を向上することができる昇華精製装置を提供することを目的とする。   Then, this invention solves the said conventional subject, and it aims at providing the sublimation refinement | purification apparatus which can improve the purity and yield of a sublimation refinement | purification substance by heating a to-be-treated substance uniformly. To do.

そして、この目的を達成するために、本発明は、昇華精製管内において、被処理物質加熱容器を揺動することで、被処理物質加熱容器に充填されている被処理物質を撹拌する昇華精製装置としたものであり、被処理物質加熱容器の内壁面と被処理物質の接触部位を更新することにより被処理物質の不均一な加熱を防止することができ、所期の目的を達成するものである。   In order to achieve this object, the present invention provides a sublimation purification apparatus for agitating a substance to be treated filled in a substance to be treated heating container by swinging the substance to be treated heating container in the sublimation purification tube. It is possible to prevent uneven heating of the treated substance by updating the contact area between the inner wall surface of the treated substance heating container and the treated substance, and to achieve the intended purpose. is there.

本発明によれば、昇華精製管内において被処理物質加熱容器を昇華精製管の内壁に沿った状態で揺動するので、被処理物質加熱容器の内部に充填された粉体状の被処理物質について、表面層と底層を入れ替えることができる。   According to the present invention, since the substance heating container to be treated is swung along the inner wall of the sublimation purification pipe in the sublimation purification pipe, the powdery substance to be treated filled in the substance heating container is processed. The surface layer and the bottom layer can be interchanged.

したがって、被処理物質と被処理物質加熱容器との接触部分において被処理物質が局所的な高温状態になることが無くなるので、被処理物質加熱容器内で不純物が形成されることを防止し、昇華精製物質の純度および収率を向上することができるという効果を得ることができる。   Accordingly, since the processed material does not reach a local high temperature state at the contact portion between the processed material and the processed material heating container, impurities are prevented from being formed in the processed material heating container, and sublimation is achieved. The effect that the purity and yield of the purified substance can be improved can be obtained.

本発明の実施の形態１の昇華精製装置の概略断面図Schematic sectional view of the sublimation purification apparatus of Embodiment 1 of the present invention 本発明の実施の形態１の昇華精製装置の被処理物質加熱容器の概略斜視図Schematic perspective view of a substance heating container to be processed in the sublimation purification apparatus according to Embodiment 1 of the present invention. 本発明の実施の形態２の昇華精製装置の概略断面図Schematic sectional view of the sublimation purification apparatus of Embodiment 2 of the present invention 本発明の実施の形態２の昇華精製装置の被処理物質加熱容器の概略斜視図The schematic perspective view of the to-be-processed substance heating container of the sublimation purification apparatus of Embodiment 2 of this invention 本発明の実施の形態３の昇華精製装置の概略断面図Schematic sectional view of a sublimation purification apparatus according to Embodiment 3 of the present invention. 本発明の実施の形態３の昇華精製装置の被処理物質加熱容器の概略斜視図The schematic perspective view of the to-be-processed substance heating container of the sublimation purification apparatus of Embodiment 3 of this invention 従来の昇華精製装置の概略断面図Schematic sectional view of a conventional sublimation purification device 従来の昇華精製装置の被処理物質加熱容器の概略斜視図Schematic perspective view of the material heating container of the conventional sublimation purification apparatus

本発明の請求項１記載の昇華精製装置は、一ヶ所以上の開口部を有する昇華精製管と減圧手段と加熱手段と被処理物質加熱容器を備え、前記減圧手段により減圧した前記昇華精製管の内部において、前記加熱手段により被処理物質加熱容器を加熱することで被処理物質加熱容器内の被処理物質を昇華させ、前記昇華精製管の内壁面に、昇華された前記被処理物質を凝結させる昇華精製装置であって、揺動手段により前記被処理物質加熱容器を揺動させることで被処理物質を撹拌する昇華精製装置である。   The sublimation purification apparatus according to claim 1 of the present invention includes a sublimation purification tube having one or more openings, a decompression unit, a heating unit, and a substance heating container, and the sublimation purification tube decompressed by the decompression unit. Inside, the target substance heating container is heated by the heating means to sublimate the target substance in the target substance heating container, and the sublimated target substance is condensed on the inner wall surface of the sublimation purification tube. The sublimation purification apparatus is a sublimation purification apparatus that stirs a target substance by swinging the target substance heating container with a swinging means.

これにより被処理物質加熱容器内部に充填された被処理物質を揺動撹拌することで均一に加熱することが可能となるので、被処理物質が局所的な高温状態になることが無くなり、不純物の生成を防止することができ、被処理物質加熱容器内で不純物が形成されることを防止し、昇華精製物質の純度および収率を向上することができるという効果を奏する。   As a result, it becomes possible to uniformly heat the substance to be treated, which is filled in the substance to be treated heating container, by shaking and agitating it. The production can be prevented, impurities are prevented from being formed in the heated substance to be treated, and the purity and yield of the sublimation purification substance can be improved.

また、前記昇華精製管の内部に一つ以上の揺動可能な捕集管を備え、前記加熱手段により被処理物質加熱容器を加熱することで被処理物質加熱容器内の被処理物質を昇華させ、前記捕集管の内壁面に、昇華された前記被処理物質を凝結させる昇華精製装置であって、捕集管と被処理物質加熱容器を連結した状態で、揺動手段により捕集管を揺動させることで被処理物質を撹拌する昇華精製装置という構成にしてもよい。   Further, the sublimation purification pipe is provided with one or more swingable collection pipes, and the target substance in the target substance heating container is sublimated by heating the target substance heating container by the heating means. A sublimation purification device for condensing the sublimated material to be treated on the inner wall surface of the collection tube, wherein the collection tube is connected by a swinging means in a state in which the collection tube and the material to be treated are heated. You may make it the structure of the sublimation purification apparatus which stirs a to-be-processed substance by making it rock | fluctuate.

これにより捕集管に連結した状態の被処理物質加熱容器内部に充填された被処理物質を揺動撹拌することで均一に加熱することが可能となるので、被処理物質が局所的な高温状態になることが無くなり、不純物の生成を防止することができ、被処理物質加熱容器内で不純物が形成されることを防止し、昇華精製物質の純度および収率を向上することができるという効果を奏する。   As a result, it becomes possible to uniformly heat the substance to be treated filled in the substance to be treated heating container connected to the collection tube by rocking and stirring, so that the substance to be treated is in a locally high temperature state. The generation of impurities can be prevented, impurities can be prevented from being formed in the heated substance to be treated, and the purity and yield of the sublimation purification substance can be improved. Play.

また、前記被処理物質加熱容器を回転させることで被処理物質を撹拌する昇華精製装置という構成にしてもよい。   Moreover, you may make it the structure of the sublimation purification apparatus which stirs a to-be-processed substance by rotating the said to-be-processed substance heating container.

これにより被処理物質加熱容器内部に充填された被処理物質を回転しながら撹拌することで均一に加熱することが可能となるので、被処理物質が局所的な高温状態になることが無くなり、不純物の生成を防止することができ、被処理物質加熱容器内で不純物が形成されることを防止し、昇華精製物質の純度および収率を向上することができるという効果を奏する。   As a result, it becomes possible to uniformly heat the substance to be treated filled in the substance to be treated heating container by rotating it while rotating, so that the substance to be treated does not become a local high temperature state, and impurities It is possible to prevent the formation of impurities, to prevent impurities from being formed in the heated substance to be treated, and to improve the purity and yield of the sublimation purification substance.

また、内部を減圧した昇華精製管内で被処理物質を加熱することにより昇華させ、前記昇華精製管の内壁面に昇華した前記被処理物質を凝結させる昇華精製方法であって、前記昇華精製管内で、前記被処理物質を揺動撹拌する昇華精製方法としてもよい。   In addition, a sublimation purification method in which a substance to be treated is sublimated by heating in a sublimation purification pipe whose inside is reduced in pressure, and the substance to be treated sublimated on an inner wall surface of the sublimation purification pipe is condensed in the sublimation purification pipe. A sublimation purification method in which the substance to be treated is shaken and stirred may be employed.

これにより被処理物質を揺動撹拌することで均一に加熱することが可能となるので、被処理物質が局所的な高温状態になることが無くなり、不純物の生成を防止することができ、被処理物質加熱容器内で不純物が形成されることを防止し、昇華精製物質の純度および収率を向上することができるという効果を奏する。   As a result, it becomes possible to uniformly heat the substance to be treated by rocking and stirring, so that the substance to be treated does not become a local high temperature state, and generation of impurities can be prevented. Impurities are prevented from being formed in the substance heating container, and the purity and yield of the sublimation purification substance can be improved.

以下、本発明の実施の形態について、図面を参照しながら説明する。   Hereinafter, embodiments of the present invention will be described with reference to the drawings.

（実施の形態１）
図１に実施の形態１の昇華精製装置の概略断面図を示す。昇華精製装置１は昇華精製管２と減圧手段３と加熱手段４ａ、４ｂ、４ｃとフランジ５ａ、５ｂからなる。昇華精製管２は長手方向の両端に開口部を有する円筒状の形状をしており、加熱手段４ａ、４ｂ、４ｃは中心に開口部を有するドーナツ形状をしており、昇華精製管２の外周部を連続的に覆い、昇華精製管２に密着するように配置されている。 (Embodiment 1)
FIG. 1 shows a schematic cross-sectional view of the sublimation purification apparatus of the first embodiment. The sublimation purification apparatus 1 includes a sublimation purification pipe 2, a decompression means 3, heating means 4a, 4b and 4c, and flanges 5a and 5b. The sublimation purification pipe 2 has a cylindrical shape with openings at both ends in the longitudinal direction, and the heating means 4a, 4b, 4c have a donut shape with an opening at the center, and the outer periphery of the sublimation purification pipe 2 The parts are continuously covered and are arranged in close contact with the sublimation purification tube 2.

昇華精製管２の長手方向両端の開口部には、フランジ５ａ、５ｂが固定されており、フランジ５ｂは流出口６を備えている。途中の配管は省略しているが、フランジ５ｂの流出口６は減圧手段３と接続されている。   Flange 5a, 5b is being fixed to the opening part of the longitudinal direction both ends of the sublimation refinement | purification pipe 2, and the flange 5b is provided with the outflow port 6. FIG. Although piping in the middle is omitted, the outlet 6 of the flange 5 b is connected to the decompression means 3.

昇華精製管２の内部には被処理物質加熱容器７が設置され、被処理物質加熱容器７には被処理物質８が充填されている。さらに、被処理物質加熱容器７は揺動軸９により揺動手段１０と連結されている。加熱手段４ａ、４ｂ、４ｃは電熱線１１を内蔵している。   A to-be-treated substance heating container 7 is installed inside the sublimation purification tube 2, and the to-be-treated substance heating container 7 is filled with a to-be-treated substance 8. Further, the substance heating container 7 is connected to the swinging means 10 by the swinging shaft 9. The heating means 4a, 4b, 4c have a heating wire 11 built-in.

被処理物質８はトリス（８−キノリノラト）アルミニウムなどの有機ＥＬに用いる有機色素や、ペンタセンなどの有機半導体である。   The substance 8 to be treated is an organic dye used for organic EL such as tris (8-quinolinolato) aluminum or an organic semiconductor such as pentacene.

図２に示すように、被処理物質加熱容器７の底面は昇華精製管２の内壁面に密着するように湾曲している。また、被処理物質加熱容器７の上面は、被処理物質加熱容器７を加熱した際に被処理物質８が効率良く昇華できるように広い開口部を有している。被処理物質加熱容器７は揺動軸９と連結されている。   As shown in FIG. 2, the bottom surface of the substance heating container 7 is curved so as to be in close contact with the inner wall surface of the sublimation purification tube 2. Further, the upper surface of the target substance heating container 7 has a wide opening so that the target substance 8 can be sublimated efficiently when the target substance heating container 7 is heated. The substance heating container 7 is connected to the swing shaft 9.

上記構成において、減圧手段３により減圧した昇華精製管２の内部において、加熱手段４ａの電熱線１１に通電すると被処理物質加熱容器７が加熱されるので被処理物質８が昇華する。加熱手段４ｃにおいては被処理物質８の昇華温度よりもわずかに低い温度で昇華精製管２を加熱している。   In the above configuration, when the heating wire 11 of the heating means 4a is energized inside the sublimation purification tube 2 decompressed by the decompression means 3, the treatment substance heating container 7 is heated, so that the treatment substance 8 is sublimated. In the heating means 4c, the sublimation purification tube 2 is heated at a temperature slightly lower than the sublimation temperature of the substance 8 to be treated.

被処理物質加熱容器７で昇華された被処理物質８は昇華精製管２の内部を拡散し、昇華精製管２の内壁面の温度が被処理物質８の昇華温度すなわち凝結温度よりも低い場所で昇華精製管２の内壁面に凝結する。   The to-be-treated material 8 sublimated in the to-be-treated material heating container 7 diffuses inside the sublimation purification tube 2, and the temperature of the inner wall surface of the sublimation purification tube 2 is lower than the sublimation temperature of the to-be-treated material 8, that is, the condensation temperature. It condenses on the inner wall surface of the sublimation purification tube 2.

本実施の形態の昇華精製装置においては、先に示したように、加熱手段４ｃの内側の昇華精製管２の内壁面が被処理物質８の昇華温度よりも低いので、凝結した成分を昇華精製物質１２として回収することができる。   In the sublimation purification apparatus of the present embodiment, as shown above, since the inner wall surface of the sublimation purification pipe 2 inside the heating means 4c is lower than the sublimation temperature of the substance 8 to be treated, the condensed components are purified by sublimation. It can be recovered as substance 12.

本発明の実施の形態で昇華精製する被処理物質８はトリス（８−キノリノラト）アルミニウムなどの有機ＥＬに用いる有機色素や、ペンタセンなどの有機半導体であり、減圧下において昇華する特性を有するものであれば、他の有機化合物についても同様の効果を得ることができ、昇華精製物質１２としては、被処理物質８を高純度化したものが得られる。   The substance to be treated 8 to be sublimated and purified in the embodiment of the present invention is an organic dye used for organic EL such as tris (8-quinolinolato) aluminum or an organic semiconductor such as pentacene, and has a property of sublimating under reduced pressure. If it exists, the same effect can be acquired also about another organic compound, and what purified the to-be-processed substance 8 as the sublimation refinement | purification substance 12 is obtained.

さらに、揺動手段１０の作用により揺動軸９を左右にねじると被処理物質加熱容器７はその底面を昇華精製管２の内壁面に密着したまま揺動することができる。すなわち揺動軸９と昇華精製管２の長手方向の回転中心軸は一致しているものである。   Further, when the rocking shaft 9 is twisted left and right by the action of the rocking means 10, the to-be-treated substance heating container 7 can be rocked with its bottom surface being in close contact with the inner wall surface of the sublimation purification tube 2. In other words, the swing axis 9 and the rotation center axis in the longitudinal direction of the sublimation purification tube 2 coincide with each other.

被処理物質加熱容器７にはその内部に被処理物質８が充填されているので、被処理物質加熱容器７が揺動軸９を中心に左右それぞれ９０度程度の回転角を示す揺動動作を加えることにより、被処理物質８の表面層と底層を入れ替えることができる。   Since the substance to be treated heating container 7 is filled with the substance to be treated 8, the substance to be treated heating container 7 performs a swinging operation that shows a rotation angle of about 90 degrees on the left and right about the swing shaft 9. By adding, the surface layer and bottom layer of the to-be-processed substance 8 can be replaced.

加熱手段４ａからの熱エネルギーは昇華精製管２を透過して、被処理物質加熱容器７に伝達され、被処理物質加熱容器７の表面から被処理物質８に伝達されるものである。揺動動作により被処理物質８表面層と底層を入れ替えることにより、被処理物質８を均一に加熱することができるものである。   The heat energy from the heating means 4a is transmitted through the sublimation purification tube 2 and transmitted to the target substance heating container 7, and is transmitted from the surface of the target substance heating container 7 to the target substance 8. By replacing the surface layer and the bottom layer of the substance to be treated 8 by the swinging operation, the substance to be treated 8 can be heated uniformly.

本実施の形態では従来の昇華精製装置と異なり、被処理物質８を均一に加熱できることから被処理物質８が局所的に昇華温度を超えて加熱されることが無くなり、被処理物質８の分解生成物である不純物が生成されることを防止し、昇華精製物質の純度および収率を向上することができる。   In the present embodiment, unlike the conventional sublimation purification apparatus, the material to be treated 8 can be heated uniformly, so that the material to be treated 8 is not locally heated above the sublimation temperature, and the material to be treated 8 is decomposed and produced. It is possible to prevent the production of impurities and improve the purity and yield of the sublimation purification material.

なお、本実施の形態では被処理物質加熱容器７を揺動する際の回転角を９０度程度と示したが、この角度に限ったものではなく、被処理物質加熱容器７の内部に充填された被処理物質８が十分に撹拌される回転角であれば、９０度以下の角度でも同様の効果を得ることができる。   In this embodiment, the rotation angle when swinging the substance heating container 7 is about 90 degrees. However, the angle is not limited to this, and the inside of the substance heating container 7 is filled. If the rotation angle at which the substance 8 to be treated is sufficiently stirred is used, the same effect can be obtained even at an angle of 90 degrees or less.

また、被処理物質加熱容器７を揺動することにより、被処理物質８が粉状のまま被処理物質加熱容器７を逸脱することは防止すべきであり、そのような状態に陥らない揺動を実施すればよい。   Further, by swinging the target substance heating container 7, it should be prevented that the target substance 8 deviates from the target substance heating container 7 in a powdery state, and the swing does not fall into such a state. Should be implemented.

なお、本実施の形態では揺動軸９はフランジ５ａを貫通している状態を示したが、昇華精製作業においては昇華精製管２の内部を真空に保つ必要があり、フランジ５ａに揺動手段１０を取り付けて揺動軸９を貫通させても真空度が低下しないよう、揺動手段１０は真空装置に一般的に適用される回転導入機を用いることが望ましい。   In this embodiment, the oscillating shaft 9 is shown penetrating the flange 5a. However, in the sublimation purification operation, it is necessary to keep the inside of the sublimation purification pipe 2 in a vacuum, and the oscillating means is attached to the flange 5a. It is desirable to use a rotation introducing machine generally applied to a vacuum apparatus as the rocking means 10 so that the degree of vacuum does not decrease even if the rocking shaft 9 is penetrated by attaching 10.

なお、回転導入機を利用した場合には、被処理物質加熱容器７内の被処理物質８が被処理物質加熱容器７から逸脱しないような回転角度と回転速度で往復揺動することで、同様の効果を得ることができる。   In the case of using a rotation introducing machine, the same is achieved by reciprocatingly swinging at a rotation angle and a rotation speed so that the substance to be treated 8 in the substance to be treated heating container 7 does not deviate from the substance to be treated heating container 7. The effect of can be obtained.

また、本実施の形態では、昇華精製物質１２は加熱手段４ｃの内側の昇華精製管２の内壁面に凝結するものとしたが、その凝結場所はその場所に限定するものではなく、凝結させたい部位の近傍の温度が被処理物質８の昇華温度すなわち凝結温度よりも低くなるように、加熱手段４ｂ、４ｃの温度を設定すればよく、加熱手段４ｂの内側の昇華精製管２の内壁面に昇華精製物質１２を凝結させても同様の効果を得ることができる。   Further, in the present embodiment, the sublimation purification substance 12 condenses on the inner wall surface of the sublimation purification pipe 2 inside the heating means 4c, but the condensing place is not limited to that place, and it is desired to condense. The temperature of the heating means 4b and 4c may be set so that the temperature in the vicinity of the site is lower than the sublimation temperature of the substance 8 to be treated, that is, the condensation temperature, and is formed on the inner wall surface of the sublimation purification pipe 2 inside the heating means 4b. Even if the sublimation purification substance 12 is condensed, the same effect can be obtained.

また、本実施の形態では昇華精製物質１２の回収方法について、特に限定しなかったが、被処理物質加熱容器７の内部に充填した被処理物質８が全て昇華された段階で、減圧手段３の運転を停止して、昇華精製管２の内部が常温常圧になった時点でフランジ５ｂを外して、昇華精製管２の開口部からスパーテル（薬さじ）等を挿入して、昇華精製物質１２を掻きだしても良い。   In the present embodiment, the method for recovering the sublimation purification substance 12 is not particularly limited. However, at the stage where all the target substances 8 filled in the target substance heating container 7 are sublimated, the decompression means 3 When the operation is stopped and the inside of the sublimation purification tube 2 reaches room temperature and normal pressure, the flange 5b is removed, and a spatula or the like is inserted from the opening of the sublimation purification tube 2 to obtain the sublimation purification material 12 May be scraped.

さらには、昇華精製管２の内部が常温常圧になった時点でフランジ５ａ、５ｂ、加熱手段４ａ、４ｂ、４ｃを昇華精製管２から取り外し、昇華精製管２の昇華精製物質１２が凝結している部位の近傍で、昇華精製管２を切断してから昇華精製物質１２を回収してもよい。   Furthermore, when the inside of the sublimation purification tube 2 reaches room temperature and normal pressure, the flanges 5a, 5b and the heating means 4a, 4b, 4c are removed from the sublimation purification tube 2, and the sublimation purification material 12 in the sublimation purification tube 2 is condensed. The sublimation purification material 12 may be recovered after the sublimation purification tube 2 is cut in the vicinity of the portion where the sublimation purification is performed.

また、本実施の形態では加熱手段４ａ、４ｂ、４ｃは電熱線１１を備えているとしたが、この構成に限ったものではなく、昇華精製管２の外部から昇華精製管２に密着した状態で加熱できるような構造であればリボンヒーター等を昇華精製管２に巻きつけて加熱しても同様の効果を得ることが可能である。   Further, in the present embodiment, the heating means 4a, 4b, and 4c are provided with the heating wire 11. However, the heating means 4a, 4b, and 4c are not limited to this configuration, but are in close contact with the sublimation purification tube 2 from the outside of the sublimation purification tube 2. The same effect can be obtained even when a ribbon heater or the like is wound around the sublimation purification tube 2 and heated if the structure can be heated by heating.

また、本実施の形態では被処理物質加熱容器７の材質について特に限定しなかったが、昇華精製管２と密着しつつ揺動可能であることが必要であり、加熱時の変形を避けるために、昇華精製管２と同じく熱膨張係数の低い材料である石英製を用いることが望ましい。   In the present embodiment, the material of the substance heating container 7 to be treated is not particularly limited. However, it is necessary to be able to swing while being in close contact with the sublimation purification pipe 2, and in order to avoid deformation during heating. As in the sublimation purification tube 2, it is desirable to use quartz which is a material having a low thermal expansion coefficient.

また、本実施の形態では減圧手段３の構造について特に限定しなかったが、ロータリーポンプ、ダイアフラムポンプ、ディフュージョンポンプ、ターボ分子ポンプなど、昇華精製管２の内部を１０-4Ｐａ程度まで減圧できるような能力を有する真空ポンプであればどのような真空ポンプでもよく、複数の真空ポンプを組み合わせて使用しても同様の効果を得ることが可能である。 In the present embodiment, the structure of the decompression means 3 is not particularly limited, but the interior of the sublimation purification pipe 2 can be decompressed to about 10 −4 Pa, such as a rotary pump, a diaphragm pump, a diffusion pump, and a turbo molecular pump. Any vacuum pump may be used as long as it has a sufficient capability, and the same effect can be obtained even when a plurality of vacuum pumps are used in combination.

（実施の形態２）
図３に実施の形態２の昇華精製装置の概略断面図を示す。図１から図２と同様の構成要素については同一の符号を付し、その詳細な説明は省略する。 (Embodiment 2)
FIG. 3 shows a schematic cross-sectional view of the sublimation purification apparatus of the second embodiment. The same components as those in FIGS. 1 to 2 are denoted by the same reference numerals, and detailed description thereof is omitted.

昇華精製装置１は昇華精製管２の内部に被処理物質加熱容器７と捕集管１３ａ、１３ｂ、１３ｃを備えている。また、昇華精製管２の周囲に、中央に開口部を有する揺動手段１４が昇華精製管２と密着するように昇華精製管２の周囲に配置されている。揺動手段１４の内部には電磁コイル１５が備えられている。   The sublimation purification apparatus 1 is provided with a substance heating container 7 and collection tubes 13a, 13b, 13c inside a sublimation purification tube 2. A swinging means 14 having an opening at the center is arranged around the sublimation purification tube 2 so as to be in close contact with the sublimation purification tube 2. An electromagnetic coil 15 is provided inside the swinging means 14.

図４に捕集管１３ａ、１３ｂ、１３ｃと被処理物質加熱容器７の概略斜視図を示す。図４に示すように捕集管１３ａ、１３ｂ、１３ｃと被処理物質加熱容器７は連結手段１６により連結されている。連結された状態では昇華精製管２の長さと同一である。   FIG. 4 shows a schematic perspective view of the collection tubes 13a, 13b, 13c and the substance heating container 7 to be treated. As shown in FIG. 4, the collection tubes 13 a, 13 b, 13 c and the substance heating container 7 are connected by a connecting means 16. In the connected state, it is the same as the length of the sublimation purification tube 2.

被処理物質加熱容器７は流出口１７を備えており、捕集管１３ｃは流出口１８を備えており、捕集管１３ｃの流出口１８と反対側の端面は開口している。捕集管１３ｂ、１３ａの両端はそれぞれ開口している。したがって、被処理物質加熱容器７と捕集管１３ｃの流出口１８は連通している。捕集管１３ｃの流出口１８は、フランジ５ｂの流出口６と連通しており、流出口６は減圧手段３と接続されている。捕集管１３ｃの表面には磁性体１９が貼付されている。   The to-be-processed substance heating container 7 is equipped with the outflow port 17, the collection pipe | tube 13c is equipped with the outflow port 18, and the end surface on the opposite side to the outflow port 18 of the collection pipe | tube 13c is opening. Both ends of the collection tubes 13b and 13a are opened. Therefore, the to-be-processed substance heating container 7 and the outflow port 18 of the collection pipe | tube 13c are connecting. The outlet 18 of the collection tube 13 c communicates with the outlet 6 of the flange 5 b, and the outlet 6 is connected to the decompression means 3. A magnetic body 19 is affixed to the surface of the collection tube 13c.

上記構成において、実施の形態１と同様に被処理物質加熱容器７に被処理物質８を充填した後に被処理物質加熱容器７を加熱すると、被処理物質８が昇華され、加熱手段４ｃの内側の捕集管１３ｂの内壁面が被処理物質８の昇華温度よりも低いので、凝結した成分を昇華精製物質１２として回収することができる。   In the above configuration, as in the first embodiment, when the target substance heating container 7 is heated after the target substance heating container 7 is filled with the target substance heating container 7, the target substance 8 is sublimated, and the inside of the heating means 4c. Since the inner wall surface of the collection tube 13b is lower than the sublimation temperature of the material 8 to be treated, the condensed components can be recovered as the sublimation purification material 12.

さらに、揺動手段１４の作用により、電磁コイル１５で回転磁界を生成すると、捕集管１３ｃの表面の磁性体１９が磁力により吸引され、捕集管１３ｃが揺動する。捕集管１３ｃ、捕集管１３ｂ、捕集管１３ａ、被処理物質加熱容器７は、連結手段１６により連結されているので、捕集管１３ｃの揺動に合わせて被処理物質加熱容器７も揺動する。   Further, when a rotating magnetic field is generated by the electromagnetic coil 15 by the action of the swinging means 14, the magnetic body 19 on the surface of the collecting tube 13c is attracted by the magnetic force, and the collecting tube 13c is swung. Since the collection tube 13c, the collection tube 13b, the collection tube 13a, and the target substance heating container 7 are connected by the connecting means 16, the target substance heating container 7 is also adapted to the swinging of the collection pipe 13c. Swing.

被処理物質加熱容器７にはその内部に被処理物質８が充填されているので、被処理物質加熱容器７に９０度程度の回転角を示す揺動動作を加えることにより、被処理物質８の表面層と底層を入れ替えることができる。   Since the material to be treated heating container 7 is filled with the material to be treated 8, the material to be treated 8 is subjected to a rocking motion showing a rotation angle of about 90 degrees. The surface layer and the bottom layer can be interchanged.

加熱手段４ａからの熱エネルギーは昇華精製管２を透過して、被処理物質加熱容器７に伝達され、被処理物質加熱容器７の表面から被処理物質８に伝達されるものである。揺動動作により被処理物質８表面層と底層を入れ替えることにより、被処理物質８を均一に加熱することができるものである。   The heat energy from the heating means 4a is transmitted through the sublimation purification tube 2 and transmitted to the target substance heating container 7, and is transmitted from the surface of the target substance heating container 7 to the target substance 8. By replacing the surface layer and the bottom layer of the substance to be treated 8 by the swinging operation, the substance to be treated 8 can be heated uniformly.

なお、本実施の形態では、昇華精製管２の内部に、捕集管１３ｃ、捕集管１３ｂ、捕集管１３ａ、被処理物質加熱容器７を連結して備えるとしたが、この構成に限ったものではなく、昇華精製管２の長軸方向について、捕集管１３ｃ、捕集管１３ｂ、捕集管１３ａ、被処理物質加熱容器７と昇華精製管２の位置が変動する事が無いように揺動可能な状態で固定されていればよく、捕集管１３ｃ、捕集管１３ｂ、捕集管１３ａの分割数について特に制限を設けるものではない。   In the present embodiment, the sublimation purification pipe 2 is provided with the collection pipe 13c, the collection pipe 13b, the collection pipe 13a, and the material heating container 7 to be treated. However, the present invention is not limited to this configuration. However, the positions of the collection tube 13c, the collection tube 13b, the collection tube 13a, the heated substance to be treated 7 and the sublimation purification tube 2 do not change in the major axis direction of the sublimation purification tube 2. As long as it is fixed in a swingable manner, the number of divisions of the collection tube 13c, the collection tube 13b, and the collection tube 13a is not particularly limited.

（実施の形態３）
図５に実施の形態３の昇華精製装置の概略断面図を示す。図１から図４と同様の構成要素については同一の符号を付し、その詳細な説明は省略する。 (Embodiment 3)
FIG. 5 shows a schematic cross-sectional view of the sublimation purification apparatus of the third embodiment. The same components as those in FIGS. 1 to 4 are denoted by the same reference numerals, and detailed description thereof is omitted.

フランジ５ａには流入口２０が備えられており、途中の配管は省略しているが、フランジ５ａの流入口２０は不活性ガス供給手段２１と接続されている。   The inflow port 20 is provided in the flange 5a, and piping in the middle is omitted, but the inflow port 20 of the flange 5a is connected to the inert gas supply means 21.

また、実施の形態２と同様に、昇華精製管２の周囲に、中央に開口部を有する揺動手段１４が昇華精製管２と密着するように昇華精製管２の周囲に配置されている。揺動手段１４の内部には電磁コイル１５が備えられている。   Similarly to the second embodiment, the swinging means 14 having an opening at the center is arranged around the sublimation purification tube 2 so as to be in close contact with the sublimation purification tube 2. An electromagnetic coil 15 is provided inside the swinging means 14.

図６に捕集管１３ａ、１３ｂ、１３ｃと被処理物質加熱容器７の概略斜視図を示す。図６に示すように被処理物質加熱容器７は流入口２２を有しており、フランジ５ａの流入口２０と連通するものである。   FIG. 6 shows a schematic perspective view of the collection tubes 13a, 13b, 13c and the substance heating container 7 to be treated. As shown in FIG. 6, the to-be-treated substance heating container 7 has the inflow port 22, and is connected with the inflow port 20 of the flange 5a.

上記構成において、実施の形態２と同様に被処理物質加熱容器７に被処理物質８を充填した後に被処理物質加熱容器７を加熱すると、被処理物質８が昇華され、加熱手段４ｃの内側の捕集管１３ｂの内壁面が被処理物質８の昇華温度よりも低いので、凝結した成分を昇華精製物質１２として回収することができる。   In the above configuration, as in the second embodiment, when the target substance heating container 7 is heated after the target substance heating container 7 is filled with the target substance heating container 7, the target substance 8 is sublimated, and the inside of the heating means 4c is increased. Since the inner wall surface of the collection tube 13b is lower than the sublimation temperature of the material 8 to be treated, the condensed components can be recovered as the sublimation purification material 12.

さらに、揺動手段１４の作用により、電磁コイル１５で回転磁界を生成すると、捕集管１３ｃの表面の磁性体１９が磁力により吸引され、捕集管１３ｃが揺動する。捕集管１３ｃ、捕集管１３ｂ、捕集管１３ａ、被処理物質加熱容器７は、連結手段１６により連結されているので、捕集管１３ｃの揺動に合わせて被処理物質加熱容器７も揺動する。   Further, when a rotating magnetic field is generated by the electromagnetic coil 15 by the action of the swinging means 14, the magnetic body 19 on the surface of the collecting tube 13c is attracted by the magnetic force, and the collecting tube 13c is swung. Since the collection tube 13c, the collection tube 13b, the collection tube 13a, and the target substance heating container 7 are connected by the connecting means 16, the target substance heating container 7 is also adapted to the swinging of the collection pipe 13c. Swing.

被処理物質加熱容器７にはその内部に被処理物質８が充填されているので、被処理物質加熱容器７に９０度程度の回転角を示す揺動動作を加えることにより、被処理物質８の表面層と底層を入れ替えることができる。加熱手段４ａからの熱エネルギーは昇華精製管２を透過して、被処理物質加熱容器７に伝達され、被処理物質加熱容器７の表面から被処理物質８に伝達されるものである。揺動動作により被処理物質８表面層と底層を入れ替えることにより、被処理物質８を均一に加熱することができるものである。   Since the material to be treated heating container 7 is filled with the material to be treated 8, the material to be treated 8 is subjected to a rocking motion showing a rotation angle of about 90 degrees. The surface layer and the bottom layer can be interchanged. The heat energy from the heating means 4a is transmitted through the sublimation purification tube 2 and transmitted to the target substance heating container 7, and is transmitted from the surface of the target substance heating container 7 to the target substance 8. By replacing the surface layer and the bottom layer of the substance to be treated 8 by the swinging operation, the substance to be treated 8 can be heated uniformly.

本実施の形態においては、昇華精製中に不活性ガス供給手段２１から微量のアルゴンガス等を供給することで、被処理物質加熱容器７内で昇華した被処理物質を流出口６の方向に向けて搬送することができる。   In the present embodiment, by supplying a small amount of argon gas or the like from the inert gas supply means 21 during sublimation purification, the substance to be sublimated in the substance heating container 7 is directed toward the outlet 6. Can be transported.

本発明にかかる昇華精製装置および昇華精製方法は、昇華精製中に被処理物質加熱容器内で不純物が形成されることを防止するものであるので、有機ＥＬや有機太陽電池または有機半導体などに使用される昇華性を有する有機化合物の精製、分離手段等として有用である。   The sublimation purification apparatus and the sublimation purification method according to the present invention are used for organic EL, organic solar cells, organic semiconductors, and the like because they prevent impurities from being formed in the heated substance to be treated during sublimation purification. It is useful as a means for purifying and separating organic compounds having sublimation properties.

１ 昇華精製装置
２ 昇華精製管
３ 減圧手段
４ａ 加熱手段
４ｂ 加熱手段
４ｃ 加熱手段
５ａ フランジ
５ｂ フランジ
６ 流出口
７ 被処理物質加熱容器
８ 被処理物質
９ 揺動軸
１０ 揺動手段
１１ 電熱線
１２ 昇華精製物質
１３ａ 捕集管
１３ｂ 捕集管
１３ｃ 捕集管
１４ 揺動手段
１５ 電磁コイル
１６ 連結手段
１７ 流出口
１８ 流出口
１９ 磁性体
２０ 流入口
２１ 不活性ガス供給手段
２２ 流入口
１０１ 昇華精製装置
１０２ 昇華精製管
１０３ 減圧手段
１０４ａ 加熱手段
１０４ｂ 加熱手段
１０４ｃ 加熱手段
１０５ａ フランジ
１０５ｂ フランジ
１０６ 流出口
１０７ 被処理物質加熱容器
１０８ 被処理物質
１０９ 電熱線
１１０ 昇華精製物質 DESCRIPTION OF SYMBOLS 1 Sublimation purification apparatus 2 Sublimation purification pipe | tube 3 Depressurization means 4a Heating means 4b Heating means 4c Heating means 5a Flange 5b Flange 6 Outflow port 7 To-be-processed substance heating container 8 To-be-processed substance 9 Swing axis 10 Swing means 11 Heating wire 12 Sublimation Purified substance 13a Collection tube 13b Collection tube 13c Collection tube 14 Oscillating means 15 Electromagnetic coil 16 Connection means 17 Outlet 18 Outlet 19 Magnetic body 20 Inlet 21 Inert gas supply means 22 Inlet 101 Sublimation purification apparatus 102 Sublimation purification tube 103 Depressurization means 104a Heating means 104b Heating means 104c Heating means 105a Flange 105b Flange 106 Outlet 107 Processed substance heating container 108 Processed substance 109 Heating wire 110 Sublimation purified substance

Claims (4)

一ヶ所以上の開口部を有する昇華精製管と減圧手段と加熱手段と被処理物質加熱容器を備え、前記減圧手段により減圧した前記昇華精製管の内部において、前記加熱手段により被処理物質加熱容器を加熱することで被処理物質加熱容器内の被処理物質を昇華させ、前記昇華精製管の内壁面に、昇華された前記被処理物質を凝結させる昇華精製装置であって、揺動手段により前記被処理物質加熱容器を揺動させることで被処理物質を撹拌する昇華精製装置。 A sublimation purification tube having one or more openings, a depressurization unit, a heating unit, and a target substance heating container, and inside the sublimation purification tube decompressed by the depressurization unit, the target substance heating container is provided by the heating unit. A sublimation purification apparatus that sublimates the target substance in the target substance heating container by heating and condenses the sublimated target substance on the inner wall surface of the sublimation purification tube, wherein A sublimation purification apparatus that stirs a substance to be treated by swinging a treatment substance heating container. 前記昇華精製管の内部に一つ以上の揺動可能な捕集管を備え、前記加熱手段により被処理物質加熱容器を加熱することで被処理物質加熱容器内の被処理物質を昇華させ、前記捕集管の内壁面に、昇華された前記被処理物質を凝結させる昇華精製装置であって、少なくとも一つの捕集管と被処理物質加熱容器を連結した状態で、揺動手段により捕集管を揺動させることで被処理物質を撹拌する昇華精製装置。 The sublimation purification tube is provided with one or more swingable collection tubes, and the target substance heating container is heated by the heating means to sublimate the target substance in the target substance heating container, A sublimation purification apparatus for condensing the sublimated material to be treated on the inner wall surface of a collection tube, wherein at least one collection tube and a material to be treated heating container are connected to each other by a swinging means. Sublimation purification device that stirs the material to be treated by swinging the sway. 前記被処理物質加熱容器を回転させることで被処理物質を撹拌する請求項１または２に記載の昇華精製装置。 The sublimation purification apparatus of Claim 1 or 2 which stirs a to-be-processed substance by rotating the said to-be-processed substance heating container. 内部を減圧した昇華精製管内で被処理物質を加熱することにより昇華させ、前記昇華精製管の内壁面に昇華した前記被処理物質を凝結させる昇華精製方法であって、
前記昇華精製管内で、前記被処理物質を揺動撹拌する昇華精製方法。 A sublimation purification method for sublimating by heating a material to be treated in a sublimation purification tube having a reduced pressure inside, and condensing the material to be treated on the inner wall surface of the sublimation purification tube,
A sublimation purification method in which the material to be treated is rocked and stirred in the sublimation purification tube.
JP2012206616A 2012-09-20 2012-09-20 Apparatus and method for sublimation purification Pending JP2014061464A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02212330A (en) * 1989-02-10 1990-08-23 Nippon Telegr & Teleph Corp <Ntt> Device and method for purifying reagent
JPH04247866A (en) * 1991-01-24 1992-09-03 Shimadzu Corp Vacuum vapor deposition device
JPH11171801A (en) * 1997-12-11 1999-06-29 Idemitsu Kosan Co Ltd Sublimation purification
JP2008543934A (en) * 2005-06-23 2008-12-04 ルーセント テクノロジーズ インコーポレーテッド Purification of organic compositions by sublimation.

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02212330A (en) * 1989-02-10 1990-08-23 Nippon Telegr & Teleph Corp <Ntt> Device and method for purifying reagent
JPH04247866A (en) * 1991-01-24 1992-09-03 Shimadzu Corp Vacuum vapor deposition device
JPH11171801A (en) * 1997-12-11 1999-06-29 Idemitsu Kosan Co Ltd Sublimation purification
JP2008543934A (en) * 2005-06-23 2008-12-04 ルーセント テクノロジーズ インコーポレーテッド Purification of organic compositions by sublimation.

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