JP5525677B2 - Purification equipment - Google Patents

Description

The present invention relates to a purification apparatus for purifying a substance and a purification method of the substance, and more particularly to an apparatus and a purification method for vaporizing and purifying a substance.

Organic compound materials such as organic electronic materials and organic semiconductor materials used for organic thin film transistors affect the characteristics and durability of the element, and therefore require high purity. Moreover, when manufacturing devices, such as a semiconductor device and a display apparatus, using an element industrially, it is calculated | required that the said organic compound material can be refine | purified efficiently in a high yield and a short time.

A sublimation purification method or the like is used as a purification method of such an organic compound material, and research has been conducted in order to efficiently purify a higher purity material (for example, see Patent Document 1). Patent Document 1 discloses a sublimation purification in which a heat source, a sublimation unit, and a collection chamber are installed in a vacuum chamber, an organic compound material provided in the sublimation unit is sublimated by heating from the heat source, and introduced into the collection chamber for collection. The method is used to efficiently purify high purity organic compound materials.
JP 2003-88704 A

To increase productivity, it is possible to increase the size of the purification equipment, but the sublimation purification method is a technology that requires precise thermal gradient control, and accurate temperature control of the purification unit may become difficult due to the increased size of the equipment. There is sex. Therefore, a technology for purifying a higher purity organic compound material with high yield and high productivity is required for mass production of devices using higher performance organic compound materials.

In view of the above problems, an object of the present invention is to provide a purification apparatus and a purification method capable of purifying a higher-purity substance with high yield and high productivity.

In the purification method of the present invention, a substance containing impurities is heated and sublimated in a system having a thermal gradient (may be under normal pressure, reduced pressure, or vacuum) (hereinafter also referred to as a purification section), and flows as a carrier gas in the system. It is a purification method in which impurities having different sublimation points and weights are separated from a target substance by transporting with an inert gas.

In the present invention, the carrier gas flowing in the system is heated before being supplied to the purification unit in the purification unit for purifying the substance, and the gas heated to a temperature close to the purification unit is supplied to the purification unit as a carrier gas. And By heating in advance, the temperature difference between the temperature of the carrier gas and the temperature of the purification unit can be reduced.

The purification method is a method for purifying a high-purity organic compound by separating impurities and an organic compound with high accuracy using a thermal gradient and a carrier gas. Therefore, precise thermal gradient control and carrier gas flow rate control are important in the purification unit.

On the other hand, as the apparatus for mass production increases in size, the purification unit for purifying the substance also increases in size. However, when the refinement part is enlarged, the heat in the refinement part system may be uneven. The heat non-uniformity in the refining unit means that the region to be maintained at the same temperature has a temperature difference, for example, due to the distance from the temperature control means (heating unit) of the refining unit. When using a tube and having temperature control means provided so as to surround the peripheral side surface of the glass tube, the temperature near the outer periphery of the glass tube near the heating unit included in the temperature control means is high, and the temperature near the center of the glass tube is Is low.

In addition, the nonuniformity of the heat in the purification unit may also be caused by the influence of the carrier gas flowing through the purification unit, which becomes more prominent due to an increase in the flow rate of the carrier gas as the apparatus becomes larger. . In order to obtain uniform heat, it is conceivable to increase the heat source of the temperature adjusting means. However, this is not only costly, but also requires a larger and more complicated device.

In the present invention, by supplying the heated carrier gas to the purification unit, it is possible to prevent temperature reduction and heat non-uniformity in the purification unit due to the carrier gas. Further, by flowing the heated carrier gas into the purification unit, the low temperature region in the enlarged purification unit can be heated and the temperature in the purification unit can be made uniform. Further, since the temperature gradient in the refined part becomes more gradual and continuous due to the heated carrier gas, the impurity and the target substance can be separated with a sufficient distance. Therefore, highly accurate fractionation can be performed and a higher-purity substance can be obtained.

One form of the purification apparatus of the present invention is a purification unit that vaporizes and purifies a substance, a purification unit temperature adjusting means that is provided in the purification unit, and that imparts a temperature gradient to the purification unit, and is provided at one end of the purification unit. Gas supply means, a gas discharge section provided at the other end of the purification section, and a gas temperature adjustment means, and the gas supplied from the gas supply means is heated by the gas temperature adjustment means and purified. Supplied to.

One form of the purifying apparatus of the present invention is provided in a purifying unit for vaporizing and purifying a substance, a temperature adjusting means for providing a temperature gradient in the purifying unit, and provided at one end of the purifying unit. A gas supply unit and a gas discharge unit provided at the other end of the purification unit are provided, and the gas supplied from the gas supply unit is heated by the temperature adjusting unit and supplied to the purification unit.

One form of the purification apparatus of the present invention is a purification unit that vaporizes and purifies a substance, a purification unit temperature adjusting means that is provided in the purification unit, and that imparts a temperature gradient to the purification unit, and is provided at one end of the purification unit. Gas supply means, a gas discharge section provided at the other end of the purification section, and a gas temperature control means, and the first gas and the second gas are supplied from the gas supply means to the purification section. The first gas supplied from the gas supply means is heated by the gas temperature adjusting means and supplied to the purification unit.

One form of the purifying apparatus of the present invention is provided in a purifying unit for vaporizing and purifying a substance, a temperature adjusting means for providing a temperature gradient in the purifying unit, and provided at one end of the purifying unit. It has a gas supply means and a gas discharge part provided at the other end of the purification section, and the first gas and the second gas are supplied from the gas supply means to the purification section and supplied from the gas supply means. The first gas is heated by the temperature adjusting means and supplied to the purification unit.

One form of the purification method of the present invention is to purify the substance by vaporizing the substance by heating the purification part provided with the substance while flowing gas from one end of the purification part to the other end in the purification part, The gas is heated before being supplied to the purification unit, the heated gas is supplied from one end of the purification unit, and the supplied gas is discharged from the other end of the purification unit.

In one form of the purification method of the present invention, the purification unit provided with the substance is heated while flowing the first gas and the second gas from one end of the purification unit to the other end in the purification unit. The substance is vaporized and purified, and the first gas is heated before being supplied to the purification unit, the heated first gas is supplied from one end of the purification unit, and the supplied first gas Is discharged from the other end of the purification unit, and the temperature of the second gas is lower than the temperature of the first gas.

The said refinement | purification part and the refinement | purification part temperature control means or temperature control means may be in contact, and may adjoin. Moreover, it may be in an integrated state. Similarly, the purification unit and the gas supply unit may be in contact with each other or may be close to each other. Note that the term “close” means a state in which the space (space) is provided to some extent.

In the above configuration, the gas (first gas, second gas) supplied to the purification unit used as the carrier gas is an inert gas (nitrogen (N ₂ ), argon (Ar), helium (He), neon ( Ne), krypton (Kr), xenon (Xe)) can be used. Further, the gas can be discharged from the gas discharge section of the purification section, and the gas discharge may be performed using a gas discharge means. As the gas discharge means, a pump such as a rotary pump or a diffusion pump may be used.

Further, the purification of the substance can be performed under normal pressure, reduced pressure, or vacuum, and the pressure in the purification unit can be controlled by a pressure gauge (vacuum gauge) while the inside of the purification unit is exhausted with a pump or the like.

In addition, the substance refine | purified by this invention shall contain in the category all the substances which can be vaporized and refine | purified. In the present specification, purification refers to the use of the three-state change of substances, and includes subdivision purification and distillation. That is, in addition to purification utilizing the phenomenon that a solid directly becomes a gas without passing through a liquid, and conversely, a phenomenon that a gas becomes a solid directly without going through a liquid, a phenomenon where a solid becomes a gas through a liquid, and Conversely, purification using the phenomenon that a gas becomes a solid through a liquid is also included. Therefore, the target substance includes not only a substance that sublimes as a solid, or condenses from a gas to a liquid, but also a substance that condenses as a liquid. In this specification, sublimation or solidification as a solid is also called precipitation.

The purification method in the present invention can be used for substances such as inorganic compound materials, organic compound materials, or mixed materials of inorganic compounds and organic compounds, and is particularly effective for organic compound materials.

In the present invention, by heating the purification unit and supplying the carrier gas with a reduced temperature difference from the purification unit, it is possible to prevent temperature reduction and heat non-uniformity in the purification unit due to the carrier gas. Further, by flowing the heated carrier gas into the purification unit, the low temperature region in the enlarged purification unit can be heated and the temperature in the purification unit can be made uniform. Further, since the temperature gradient in the refined part becomes more gradual and continuous due to the heated carrier gas, the impurity and the target substance can be separated with a sufficient distance. Therefore, highly accurate fractionation can be performed and a higher-purity substance can be obtained.

Therefore, by using the purification apparatus and the purification method of the present invention, a higher-purity substance can be purified with high yield and high productivity.

Embodiments of the present invention will be described below with reference to the drawings. However, the present invention can be implemented in many different modes, and those skilled in the art can easily understand that the modes and details can be variously changed without departing from the spirit and scope of the present invention. Is done. Therefore, the present invention is not construed as being limited to the description of this embodiment mode. Note that in all the drawings for describing the embodiments, the same portions or portions having similar functions are denoted by the same reference numerals, and repetitive description thereof is omitted.

(Embodiment 1)
In this embodiment, an example of a purification apparatus and a purification method aimed at purifying a higher-purity substance with high yield and high productivity will be described with reference to FIG.

FIG. 1A is a block diagram schematically showing the purification apparatus of the present invention, and FIG. 1B is a cross-sectional view.

The purification apparatus 100 of the present invention includes a gas supply unit 102a and a gas discharge unit 102b, a purification unit 102 for vaporizing a substance as a sample and purifying and recovering a target substance, and a purification for vaporizing and purifying the sample. Temperature control means 105, gas supply means 101 for supplying a gas as a carrier gas from the gas supply section 102a to the purification section 102, gas discharge means 103 for discharging the carrier gas from the gas discharge section 102b of the purification section 102, Gas temperature adjusting means 104 is provided for adjusting the temperature of the gas supplied from the gas supply means 101 by heating. By introducing the carrier gas from the gas supply means 101, the vaporized sample can be diffused smoothly. Note that in this specification, a sample refers to a substance in which a target substance, impurities, a solvent, and the like are mixed. In this embodiment, when the gas is exhausted from the purification unit 102, an example is shown in which the gas discharging unit 103 is used to discharge the gas from the gas discharging unit 102b. However, the gas discharging unit 103 is not necessarily used.

As shown in FIG. 1B, the purification unit temperature adjustment means 105 is provided in the vicinity of the purification unit 102, and the purification unit 102 is given a temperature gradient by the purification unit temperature adjustment means 105. Specifically, the purification unit 102 is provided with a temperature gradient so that at least the target substance can be isolated, purified, and recovered, such as a temperature range where the sample is vaporized and a temperature range where the target substance is precipitated or condensed.

The refining unit 102 and the refining unit temperature adjusting means 105 may be in contact with each other, may be close to each other, or may be integrally incorporated. Similarly, the purification unit 102 and the gas supply unit 101 may be in contact with each other, may be close to each other, or may be in an integrated state. “Adjacent” refers to a state in which the space (space) is provided to some extent.

When a metal tube such as tungsten or tantalum is used as the purification unit 102, a voltage can be applied to the metal tube and the metal tube can be heated, so that the purification unit temperature adjusting means 105 can be used.

In the present embodiment, in the purifying unit 102 for purifying a substance, the carrier gas flowing in the system is heated by the gas temperature adjusting means 104 before being supplied to the purifying unit 102, and the gas heated to a temperature close to the purifying unit 102 is changed. The carrier gas is supplied to the purification unit 102. By heating in advance, the temperature difference between the temperature of the carrier gas and the temperature of the purification unit 102 can be reduced.

The purification method is a method for purifying a high-purity organic compound by separating impurities and an organic compound with high accuracy using a thermal gradient and a carrier gas. Therefore, precise thermal gradient control and carrier gas flow rate control are important in the purification unit.

On the other hand, as the apparatus for mass production increases in size, the purification unit for purifying the substance also increases in size. However, when the refinement part is enlarged, the heat in the refinement part system may be uneven. The heat non-uniformity in the refining unit means that the region to be maintained at the same temperature has a temperature difference, for example, due to the distance from the temperature control means (heating unit) of the refining unit. When using a tube and having temperature control means provided so as to surround the peripheral side surface of the glass tube, the temperature near the outer periphery of the glass tube near the heating unit included in the temperature control means is high, and the temperature near the center of the glass tube is Is low.

In addition, the nonuniformity of the heat in the purification unit may also be caused by the influence of the carrier gas flowing through the purification unit, which becomes more prominent due to an increase in the flow rate of the carrier gas as the apparatus becomes larger. . In order to obtain uniform heat, it is conceivable to increase the heat source of the temperature adjusting means. However, this is not only costly, but also requires a larger and more complicated device.

In the present embodiment, the carrier gas that has been heated to reduce the temperature difference from the purification unit is supplied to the purification unit 102, thereby preventing temperature decrease and heat non-uniformity in the purification unit 102 due to the carrier gas. it can. In addition, by flowing the heated carrier gas into the purification unit 102, the low temperature region in the purification unit 102 that has been enlarged can be heated, and the temperature in the purification unit 102 can be made uniform. Furthermore, the heated carrier gas makes the temperature gradient in the purification unit 102 more gradual and continuous, so that the impurity and the target substance can be separated with a sufficient distance. Therefore, highly accurate fractionation can be performed and a higher-purity substance can be obtained.

For example, when pentacene, which is an organic semiconductor material, is used as a substance to be purified, the temperature at which pentacene is sublimated is about 280 ° C., and impurities are removed at about 220 ° C. In this case, since the carrier gas supplied to the purification unit may be adjusted to a temperature around 280 ° C., the heated carrier gas is preferably within ± 60 ° C. from the sublimation temperature in the purification unit.

In the above configuration, the gas supplied to the purification unit used as the carrier gas is an inert gas (nitrogen (N ₂ ), argon (Ar), helium (He), neon (Ne), krypton (Kr), xenon (Xe )) Can be used. Moreover, what is necessary is just to use a pump etc. as a discharge means.

The carrier gas introduced into the purification unit from the gas supply means may be other than an inert gas, but the inert gas is preferred because it can suppress oxidation, decomposition, etc. of the sample and the target substance. Of course, a gas that reacts with the sample or the target substance existing in the purification section must not be used.

Further, the purification of the substance can be performed under normal pressure, reduced pressure, or vacuum, and the pressure of the purification unit is controlled by a pressure gauge (vacuum gauge), and the purification unit 102 is controlled by a pump or the like used as the gas discharge means 103. What is necessary is just to exhaust the inside. Further, the gas discharge means 103 is not always necessary and may be not used under normal pressure.

What is necessary is just to connect a gas exhausting means and a refinement | purification part using piping etc. Further, a cooling trap using liquid nitrogen or the like may be provided between the purification unit and the gas discharge means. When the inside of the purification unit is depressurized by a vacuum evacuation means to be in a vacuum state, the temperature at which the sample is vaporized can be lowered. That is, when the purification unit is depressurized using the gas discharging means, the sublimation or evaporation temperature of the sample is lowered, and it is possible to vaporize a sample that does not vaporize under atmospheric pressure.

The sample vaporized in the purification unit 102 diffuses toward the lower vapor pressure. Vapor pressure generally increases with increasing temperature. Therefore, the vaporized sample diffuses toward the lower temperature according to the temperature gradient. That is, the vaporized sample is condensed as a liquid or deposited as a solid at a temperature at which the state changes to a liquid or a solid according to the pressure and temperature gradient in the purification tube. Note that the temperature region where the sample is vaporized is the hottest region of the purification unit 102. The temperature gradient may be such that the temperature decreases in one direction, or the center of the purification unit 102 may be a high temperature region, and the temperature may decrease in both directions. Also in this case, it is preferable to set the temperature of the carrier gas flowing through the purification unit to approximately the same as the set temperature of the flowing region, and the temperature of the carrier gas supplied may be set according to the setting of the temperature gradient in the purification unit 102.

The temperature setting of the carrier gas is preferably lower than the temperature at which the target substance in the material substance is altered by decomposition or the like. The temperature of the carrier gas is set so that the temperature gradient becomes gentler as the temperature is higher, and the temperature is preferably set to the same level as that of the other purification unit temperature adjusting means 105. For example, when the temperature is set lower than the temperature of the refining unit temperature adjusting means 105, the recovery area can be reduced, so that the recovery efficiency is improved.

In the case where a substance that is a material is prone to sudden boiling, it is preferable to set the setting of the refining unit temperature adjusting means 105 lower than the setting of the carrier gas so as not to bump. Then, since the substance is vaporized from the part that is in contact with the carrier gas, bumping can be prevented. Preferably, the temperature of the carrier gas gas temperature adjusting means 104 may be set to a temperature at which the substance vaporizes, and the temperature of the purification unit temperature adjusting means 105 may be set to a temperature at which the substance does not bump.

As the gas temperature adjusting unit 104 and the purification unit temperature adjusting unit 105, a heater, a hot plate, or the like may be used, and it may be provided in the vicinity of the purification unit 102 (for example, in the vicinity of the purification tube for vaporizing the sample). Although FIG. 1 shows the case where the gas temperature adjusting means 104 is provided in the gas supply means 101 and only one purifying section temperature adjusting means 105 is provided close to the purifying section 102, the present invention is not limited to this. A plurality of them may be provided. The installation location and the number of the gas temperature adjusting means 104 and the purification unit temperature adjusting means 105 can be changed as appropriate. Further, in order to keep the temperature gradient applied to the purifying unit 102 constant, protection of the heat insulating means, the metal cover surrounding the pipe through which the gas heated by the purifying unit 102 and the gas temperature adjusting means 104 passes, and glass wool, etc. It is preferable to provide a cover or the like.

When adjusting the temperature of the purification unit 102, it is necessary to set the temperature region such as the temperature at which the sample is vaporized and the temperature at which the target substance is precipitated or condensed to an optimum temperature. This may be set by examining the decomposition point, sublimation point or boiling point of the target substance.

The purification unit 102 is preferably configured by connecting two or more purification tubes. The number of purification tubes arranged in the purification unit 102 can be changed as appropriate. Specifically, it preferably includes two or more purification tubes, including a first purification tube for arranging the sample and a second purification tube for collecting the target substance that has been purified and deposited or condensed. If you do. The basic structure of the purification tube is a hollow tube. The purification tube is provided with an opening at least at the end of the adjacent purification tube so that the vaporized sample (including the target substance and impurities) can pass through. As the purification tube, it is preferable to use a hollow tube made of glass, quartz or the like. In addition, the present invention is not limited to this, and any material that does not react with the sample, the target substance, and impurities, and that can withstand the operating temperature without being mixed into the target substance when the target substance is recovered may be used. In the case of purification at normal pressure, if the purification unit 102 is sealed and heated, the pressure in the tube may increase, which is extremely dangerous. Therefore, either end must be open. Therefore, when using this refinement | purification apparatus by a normal pressure, you have to provide the opening (gas discharge part 102b) at least one place in the refinement | purification part 102 which communicates with the external environment.

Next, the refining section 102 shown in FIG. 1 is provided with a fixing means for fixing between purification steps, and at least a means capable of holding and fixing the state where the purification tubes are arranged adjacent to each other may be used. Preferably, the purification unit 102 may be a means that can be held and fixed so as to be horizontal in the long axis direction. As the fixing means, each purification tube included in the purification unit 102 may be fixed with a clamp or the like, or the purification tube may be arranged on a horizontal base. Moreover, you may arrange | position in pipes, such as glass which has a pipe inner diameter larger than the pipe outer diameter of a refinement | purification pipe | tube.

In the present embodiment, by heating the purification unit and supplying the carrier gas with a reduced temperature difference from the purification unit, it is possible to prevent temperature reduction and heat non-uniformity in the purification unit due to the carrier gas. Further, by flowing the heated carrier gas into the purification unit, the low temperature region in the enlarged purification unit can be heated and the temperature in the purification unit can be made uniform. Further, since the temperature gradient in the refined part becomes more gradual and continuous due to the heated carrier gas, the impurity and the target substance can be separated with a sufficient distance. Therefore, highly accurate fractionation can be performed and a higher-purity substance can be obtained.

Further, the purification method in this embodiment can be used for substances such as inorganic compound materials, organic compound materials, or mixed materials of inorganic compounds and organic compounds, and is particularly effective for organic compound materials.

The substance purified in this embodiment can be used for various elements such as a light-emitting element using an organic thin film transistor or an organic electroluminescence element as an example. Since the substance is purified to a high purity, the characteristics of the manufactured element can be improved.

Therefore, by using the purification apparatus and the purification method of this embodiment, a higher-purity substance can be purified with high yield and high productivity.

(Embodiment 2)
In this embodiment, an example of a purification apparatus and a purification method for purifying a higher-purity substance with high yield and high productivity will be described with reference to FIGS. In the purifying apparatus and the purifying method of the first embodiment, the means for adjusting the temperature of the gas is an example, and the same material and method may be used for the part having the same function as that of the first embodiment, and the repetition thereof Description is omitted.

FIG. 2A is a block diagram schematically showing the purification apparatus of the present invention, and FIG. 2B is a cross-sectional view.

The purification apparatus 110 according to the present embodiment includes a gas supply unit 112a and a gas discharge unit 112b, a purification unit 112 for purifying and recovering a target substance by vaporizing a substance as a sample, and a gas supply unit to the purification unit 112 A gas supply unit 111 for supplying a gas serving as a carrier gas from 112a, a gas discharge unit 113 for discharging the carrier gas from a gas discharge unit 112b of the purification unit 112, a purification unit temperature adjusting unit for vaporizing and purifying the sample, and The temperature adjusting means 114 also serves as a gas temperature adjusting means for adjusting the temperature of the gas supplied from the gas supply means 111 by heating. By introducing the carrier gas from the gas supply means 111, the vaporized sample can be diffused smoothly. In this embodiment, when the gas is exhausted from the purifying unit 112, an example is shown in which the gas discharging unit 113 is used to discharge the gas from the gas discharging unit 112b. However, the gas discharging unit 113 is not necessarily used.

The purification apparatus 110 according to the present embodiment adjusts the temperature of a purification unit temperature adjustment unit that heats to purify a substance, and a gas temperature adjustment unit that heats the carrier gas supplied from the gas supply unit 111 to the purification unit 112. The means 114 is used in common. Thus, when the temperature control means is used in common for the purifying section and the gas, the apparatus is simplified, so that the size can be reduced, the space can be saved, and the cost can be reduced. Moreover, since the refinement | purification part and the gas supplied are heated and adjusted to substantially the same temperature, even if it does not set temperature separately, the temperature of a refinement | purification part can be equalized.

As shown in FIG. 2B, the temperature adjusting unit 114 is provided in the vicinity of the purifying unit 112, and the purifying unit 112 is given a temperature gradient by the temperature adjusting unit 114. Specifically, the purification unit 112 is provided with a temperature gradient so that at least the target substance can be isolated, purified, and recovered, such as a temperature range where the sample vaporizes and a temperature range where the target substance precipitates or condenses.

The refining unit 112 and the temperature adjusting means 114 may be in contact with each other, may be close to each other, or may be in an integrated state. Similarly, the purification unit 112 and the gas supply means 111 may be in contact with each other, may be close to each other, or may be in an integrated state. Note that the term “close” means a state in which the space (space) is provided to some extent.

When a metal tube such as tungsten or tantalum is used as the purification unit 112, a voltage can be applied to the metal tube and the metal tube can be heated, so that it can be used as the temperature adjusting means 114.

In the present embodiment, in the purifying unit 112 for purifying the substance, the carrier gas flowing in the system is heated by the temperature adjusting means 114 before being supplied to the purifying unit 112, and the gas heated to a temperature close to the purifying unit 112 is used as the carrier. It supplies to the refinement | purification part 112 as gas, It is characterized by the above-mentioned. By heating in advance, the temperature difference between the temperature of the carrier gas and the temperature of the purification unit 112 can be reduced.

The purification method is a method for purifying a high-purity organic compound by separating impurities and an organic compound with high accuracy using a thermal gradient and a carrier gas. Therefore, precise thermal gradient control and carrier gas flow rate control are important in the purification unit.

On the other hand, as the apparatus for mass production increases in size, the purification unit for purifying the substance also increases in size. However, when the refinement part is enlarged, the heat in the refinement part system may be uneven. The heat non-uniformity in the refining unit means that the region to be maintained at the same temperature has a temperature difference, for example, due to the distance from the temperature control means (heating unit) of the refining unit. When using a tube and having temperature control means provided so as to surround the peripheral side surface of the glass tube, the temperature near the outer periphery of the glass tube near the heating unit included in the temperature control means is high, and the temperature near the center of the glass tube is Is low.

In addition, the nonuniformity of the heat in the purification unit may also be caused by the influence of the carrier gas flowing through the purification unit, which becomes more prominent due to an increase in the flow rate of the carrier gas as the apparatus becomes larger. . In order to obtain uniform heat, it is conceivable to increase the heat source of the temperature adjusting means. However, this is not only costly, but also requires a larger and more complicated device.

In the present embodiment, the carrier gas that has been heated to reduce the temperature difference from the purification unit is supplied to the purification unit 112, thereby preventing temperature drop and heat non-uniformity in the purification unit 112 due to the carrier gas. it can. In addition, by flowing the heated carrier gas into the purification unit 112, the low temperature region in the purification unit 112 that has been enlarged can be heated, and the temperature in the purification unit 112 can be made uniform. Further, the heated carrier gas causes the temperature gradient in the purification unit 112 to become more moderate and continuous, so that the impurity and the target substance can be separated with a sufficient distance. Therefore, highly accurate fractionation can be performed and a higher-purity substance can be obtained.

In the above configuration, the gas supplied to the purification unit used as the carrier gas is an inert gas (nitrogen (N ₂ ), argon (Ar), helium (He), neon (Ne), krypton (Kr), xenon (Xe )) Can be used. Moreover, what is necessary is just to use a pump etc. as a discharge means.

The carrier gas introduced into the purification unit from the gas supply means may be other than an inert gas, but the inert gas is preferred because it can suppress oxidation, decomposition, etc. of the sample and the target substance. Of course, a gas that reacts with the sample or the target substance existing in the purification section must not be used.

Further, the purification of the organic compound can be performed under normal pressure, reduced pressure, or vacuum, and the control of the pressure in the purification unit is controlled by a pressure gauge (vacuum gauge), and the purification unit is operated with a pump or the like used as the gas discharge means 113. What is necessary is just to exhaust the inside of 112. Further, the gas discharge means 113 is not necessarily used if it is under normal pressure, and thus it may not be used.

What is necessary is just to connect a gas exhausting means and a refinement | purification part using piping etc. Further, a cooling trap using liquid nitrogen or the like may be provided between the purification unit and the gas discharge means. When the inside of the purification unit is depressurized by a vacuum evacuation means to be in a vacuum state, the temperature at which the sample is vaporized can be lowered. That is, when the purification unit is depressurized using the gas discharging means, the sublimation or evaporation temperature of the sample is lowered, and it is possible to vaporize a sample that does not vaporize under atmospheric pressure.

The sample vaporized in the purification unit 112 diffuses toward the lower vapor pressure. Vapor pressure generally increases with increasing temperature. Therefore, the vaporized sample diffuses toward the lower temperature according to the temperature gradient. That is, the vaporized sample is condensed as a liquid or deposited as a solid at a temperature at which the state changes to a liquid or a solid according to the pressure and temperature gradient in the purification tube. Note that the temperature region where the sample is vaporized is the hottest region of the purification unit 112. The temperature gradient may be such that the temperature decreases in one direction, or the center of the purification unit 112 may be a high temperature region, and the temperature may decrease in both directions. Also in this case, it is preferable to set the temperature of the carrier gas flowing through the purification unit to approximately the same as the set temperature of the flowing region, and the temperature of the carrier gas to be supplied may be set according to the temperature gradient setting in the purification unit 112.

The temperature setting of the carrier gas is preferably lower than the temperature at which the target substance in the material substance is altered by decomposition or the like. In addition, the temperature setting of the carrier gas is preferably as high as the temperature gradient becomes gentler, and the same temperature as the other temperature control means 114, but if the target product can obtain the target purity, When the temperature is set to be lower than the temperature of the temperature adjusting means 114, the collection area can be made smaller, so that the collection efficiency is improved.

In the case where the substance that is the material is easily bumped, it is preferable to set the temperature adjusting means 114 lower than the setting of the carrier gas so as not to bump. Then, since the substance is vaporized from the part that is in contact with the carrier gas, bumping can be prevented.

As the temperature adjusting means 114, a heater, a hot plate, or the like may be used, and it may be provided in the vicinity of the purification unit 112 (for example, in the vicinity of the purification tube for vaporizing the sample). 2 shows a case where only one temperature adjusting means 114 is provided in the vicinity of the purification unit 112, the present invention is not limited to this, and a plurality of temperature adjusting means 114 may be provided. The installation location and the number of the temperature adjusting means 114 can be changed as appropriate. In addition, it is preferable to provide a heat retaining means, a protective cover surrounding a pipe through which the gas heated by the purifying section 112 and the temperature adjusting means 114 passes, or the like so that the temperature gradient applied to the purifying section 112 can be kept constant.

When adjusting the temperature of the purification unit 112, it is necessary to set the temperature region such as the temperature at which the sample is vaporized and the temperature at which the target substance is deposited or condensed to an optimum temperature. This may be set by examining the decomposition point, sublimation point or boiling point of the target substance.

The purification unit 112 is preferably configured by connecting two or more purification tubes. The number of purification tubes arranged in the purification unit 112 can be changed as appropriate. Specifically, it preferably includes two or more purification tubes, including a first purification tube for arranging the sample and a second purification tube for collecting the target substance that has been purified and deposited or condensed. If you do. The basic structure of the purification tube is a hollow tube. The purification tube is provided with an opening at least at the end of the adjacent purification tube so that the vaporized sample (including the target substance and impurities) can pass through. As the purification tube, it is preferable to use a hollow tube made of glass, quartz or the like. In addition, the present invention is not limited to this, and any material that does not react with the sample, the target substance, and impurities, and that can withstand the operating temperature without being mixed into the target substance when the target substance is recovered may be used. In the case of purification at normal pressure, if the purification unit 112 is sealed and heated, the pressure in the tube may increase, which is extremely dangerous. Therefore, either end must be open. Therefore, when using this refinement | purification apparatus by a normal pressure, you have to provide the opening (gas discharge part 112b) at least one place in the refinement | purification part 112 which communicates with the external environment.

Next, the refining section 112 shown in FIG. 2 is provided with a fixing means for fixing between purification steps, and at least a means capable of holding and fixing the state where the purification tubes are arranged adjacent to each other may be used. Preferably, the purification unit 112 may be a means that can be held and fixed so as to be horizontal in the long axis direction. As a fixing means, each purification tube included in the purification unit 112 may be fixed by a clamp or the like, or the purification tube may be arranged on a horizontal base. Moreover, you may arrange | position in pipes, such as glass which has a pipe inner diameter larger than the pipe outer diameter of a refinement | purification pipe | tube.

Further, the purification method in this embodiment can be used for substances such as inorganic compound materials, organic compound materials, or mixed materials of inorganic compounds and organic compounds, and is particularly effective for organic compound materials.

The substance purified in this embodiment can be used for various elements such as a light-emitting element using an organic thin film transistor or an organic electroluminescence element as an example. Since the substance is purified to a high purity, the characteristics of the manufactured element can be improved.

In the present embodiment, by heating the purification unit and supplying the carrier gas with a reduced temperature difference from the purification unit, it is possible to prevent temperature reduction and heat non-uniformity in the purification unit due to the carrier gas. Further, by flowing the heated carrier gas into the purification unit, the low temperature region in the enlarged purification unit can be heated and the temperature in the purification unit can be made uniform. Further, since the temperature gradient in the refined part becomes more gradual and continuous due to the heated carrier gas, the impurity and the target substance can be separated with a sufficient distance. Therefore, highly accurate fractionation can be performed and a higher-purity substance can be obtained.

Therefore, by using the purification apparatus and the purification method of this embodiment, a higher-purity substance can be purified with high yield and high productivity.

(Embodiment 3)
In this embodiment, an example of a purification device and a purification method for purifying a higher-purity substance with high yield and high productivity will be described with reference to FIGS. In the purification apparatus and the purification method of the first embodiment, the gas temperature adjusting means is an example to be described in detail, and the same material and method may be used for the portion having the same function as in the first embodiment, and the repetition thereof. Description of is omitted.

FIG. 3A is a block diagram schematically showing the purification apparatus of the present invention, and FIG. 3B is a cross-sectional view.

The purification apparatus 120 of the present invention includes a gas supply unit 122a and a gas discharge unit 122b, a purification unit 122 for vaporizing a substance as a sample and purifying and recovering a target substance, and for vaporizing and purifying the sample. A purification unit temperature adjusting unit 125; a gas supply unit 121 that supplies a gas serving as a carrier gas from the gas supply unit 122a to the purification unit 122; and a gas discharge unit 123 that discharges a carrier gas from the gas discharge unit 122b of the purification unit 122. And a gas temperature adjusting means 124 for adjusting the temperature of the gas supplied from the gas supply means 121 by heating. By introducing the carrier gas from the gas supply means 121 (121a, 121b), the vaporized sample can be diffused smoothly. In this embodiment, when the gas is exhausted from the purifying unit 122, an example is shown in which the gas exhausting unit 123 is used to exhaust the gas from the gas exhausting unit 122b. However, the gas exhausting unit 123 is not necessarily used.

As shown in FIG. 3B, the purification unit temperature adjustment means 125 is provided in the vicinity of the purification unit 122, and the purification unit 122 is given a temperature gradient by the purification unit temperature adjustment means 125. Specifically, the purification unit 122 is provided with a temperature gradient so that at least the target substance can be isolated, purified, and recovered, such as a temperature range where the sample is vaporized and a temperature range where the target substance is precipitated or condensed.

The refining part 122 and the refining part temperature adjusting means 125 may be in contact with each other, may be close to each other, or may be in an integrated state. Similarly, the purification unit 122 and the gas supply unit 121 may be in contact with each other, may be close to each other, or may be in an integrated state. “Adjacent” refers to a state in which the space (space) is provided to some extent.

When a metal tube such as tungsten or tantalum is used as the purification unit 122, a voltage can be applied to the metal tube and the metal tube can be heated, so that the purification unit temperature adjusting unit 125 can be used.

In the present embodiment, in the purification unit 122 for purifying the substance, before supplying a part of the gas supplied from the gas supply unit 121 to the purification unit 122, the gas is heated by the gas heating unit 127 of the gas temperature adjusting unit 124, A gas adjusted to a temperature close to the purification unit 122 is supplied to the purification unit 122 as a carrier gas. The temperature difference between the temperature of the carrier gas and the temperature of the purification unit 122 can be reduced by adjusting the temperature of the gas that is supplied and supplied with the preheated gas.

A method of supplying the carrier gas supplied from the gas supply unit 121 to the purification unit 122 will be described in more detail with reference to FIG. In FIG. 3B, the gas supplied from the gas supply means 121 is supplied by opening and closing cocks 129a and 129b which are stopcocks for controlling the supply amount. FIG. 3B shows an example in which the gas is supplied from the gas supply means 121 through two supply ports. However, there may be only one supply port, and the supply pipe branches to allow the gas to flow through a plurality of paths. It can also be transported.

FIG. 3C shows an example in which a plurality of gas supply means are provided and gas is supplied from each gas supply means through a supply pipe. In FIG. 3C, the second gas is supplied from the gas supply means 121a through the cock 129a, and the first gas is supplied from the gas supply means 121b through the cock 129b. The gases supplied by the gas supply means 121a and the gas supply means 121b may be different materials or the same material. In the same case, it is preferable that the gas supply unit 121a and the gas supply unit 121b are combined as shown in FIG.

The gas supplied through the cock 129b of the gas supply means 121 by the gas temperature adjusting means 124 is heated by the gas heating means 127 through the supply pipe 132 and supplied to the supply pipe 133 as a high temperature first gas. Is done. On the other hand, since the gas supplied through the cock 129a of the gas supply means 121 is not heated, it is a second gas having a temperature lower than that of the first gas. The first gas and the second gas having different temperatures are mixed and adjusted to a temperature suitable for supplying to the purification unit. A thermometer for measuring the temperature of the gas for monitoring the temperature may be provided in the supply pipe 134. The temperature-adjusted gas is supplied to the purification unit 122 through the supply pipe 134. In this way, by using a plurality of gases having different temperatures, it is possible to accurately control the temperature of the supplied gas. Further, since the respective flow rates can be appropriately controlled by the cocks 129a and 129b, the temperature control of the carrier gas can be performed more precisely. For example, the temperature of the carrier gas can be controlled appropriately in response to a temperature change of the purification unit during purification.

In the present embodiment, the carrier gas that has been heated to reduce the temperature difference from the purification unit is supplied to the purification unit 122, thereby preventing temperature drop and heat nonuniformity in the purification unit 122 due to the carrier gas. it can. In addition, by flowing the heated carrier gas into the purification unit 122, the low temperature region in the purification unit 122 that has been enlarged can be heated, and the temperature in the purification unit 122 can be made uniform. Further, since the temperature gradient in the purification unit 122 becomes more gradual and continuous due to the heated carrier gas, the impurity and the target substance can be separated with a sufficient distance. Therefore, highly accurate fractionation can be performed and a higher-purity substance can be obtained.

In the above configuration, the gas (first gas, second gas) supplied to the purification unit used as the carrier gas is an inert gas (nitrogen (N ₂ ), argon (Ar), helium (He), neon ( Ne), krypton (Kr), xenon (Xe)) can be used. Moreover, what is necessary is just to use a pump etc. as a discharge means.

The carrier gas introduced into the purification unit from the gas supply means may be other than an inert gas, but the inert gas is preferred because it can suppress oxidation, decomposition, etc. of the sample and the target substance. Of course, a gas that reacts with the sample or the target substance existing in the purification section must not be used.

Moreover, the purification of the substance can be performed under normal pressure, reduced pressure, or vacuum, and the pressure of the purification unit is controlled by a pressure gauge (vacuum gauge), and the purification unit 122 is used with a pump or the like used as the gas discharge means 123. What is necessary is just to exhaust the inside. Further, the gas discharging means 123 is not always necessary and may not be used under normal pressure.

What is necessary is just to connect a gas exhausting means and a refinement | purification part using piping etc. Further, a cooling trap using liquid nitrogen or the like may be provided between the purification unit and the gas discharge means. When the inside of the purification unit is depressurized by a vacuum evacuation means to be in a vacuum state, the temperature at which the sample is vaporized can be lowered. That is, when the purification unit is depressurized using the gas discharging means, the sublimation or evaporation temperature of the sample is lowered, and it is possible to vaporize a sample that does not vaporize under atmospheric pressure.

As the gas temperature adjusting unit 124 and the purification unit temperature adjusting unit 125 (gas heating unit 127), a heater, a hot plate or the like may be used, and it is close to the purification unit 122 (for example, in the vicinity of the purification tube for vaporizing the sample). Should be provided. 3 shows a case where only one gas temperature adjusting means 124 is provided in the gas supply means 121 and only one purification unit temperature adjusting means 125 is provided in the vicinity of the purification unit 122. However, the present invention is not limited to this. A plurality of them may be provided. The installation location and the number of the gas temperature adjusting means 124 and the purification unit temperature adjusting means 125 can be changed as appropriate. In addition, in order to keep the temperature gradient applied to the purifying unit 122 constant, a heat insulating unit, a protective cover that surrounds the supply pipes 133 and 134 through which the gas heated by the purifying unit 122 and the gas temperature adjusting unit 124 passes, etc. It is preferable to provide it.

When adjusting the temperature of the purification unit 122, it is necessary to set the temperature region such as the temperature at which the sample is vaporized and the temperature at which the target substance is precipitated or condensed to an optimum temperature. This may be set by examining the decomposition point, sublimation point or boiling point of the target substance.

The purification unit 122 is preferably configured by connecting two or more purification tubes. The number of purification tubes arranged in the purification unit 102 can be changed as appropriate. Specifically, it preferably includes two or more purification tubes, including a first purification tube for arranging the sample and a second purification tube for collecting the target substance that has been purified and deposited or condensed. If you do. The basic structure of the purification tube is a hollow tube. The purification tube is provided with an opening at least at the end of the adjacent purification tube so that the vaporized sample (including the target substance and impurities) can pass through. As the purification tube, it is preferable to use a hollow tube made of glass, quartz or the like. In addition, the present invention is not limited to this, and any material that does not react with the sample, the target substance, and impurities, and that can withstand the operating temperature without being mixed into the target substance when the target substance is recovered may be used. In the case of purification at normal pressure, if the purification unit 122 is sealed and heated, the pressure in the tube may increase, which is extremely dangerous. Therefore, either end must be open. Therefore, when using this refinement | purification apparatus by a normal pressure, you have to provide the opening (gas discharge part 122b) at least one place in the refinement | purification part 122 which communicates with the external environment.

Next, the refining unit 122 shown in FIG. 3 is provided with a fixing means for fixing between purification steps, and at least a means capable of holding and fixing the state in which the purification tubes are arranged adjacent to each other may be used. Preferably, the purification unit 122 may be a means that can be held and fixed so as to be horizontal in the long axis direction. As the fixing means, each purification tube included in the purification unit 122 may be fixed by a clamp or the like, or the purification tube may be arranged on a horizontal base. Moreover, you may arrange | position in pipes, such as glass which has a pipe inner diameter larger than the pipe outer diameter of a refinement | purification pipe | tube.

Further, the purification method in this embodiment can be used for substances such as inorganic compound materials, organic compound materials, or mixed materials of inorganic compounds and organic compounds, and is particularly effective for organic compound materials.

The substance purified in this embodiment can be used for various elements such as a light-emitting element using an organic thin film transistor or an organic electroluminescence element as an example. Since the substance is purified to a high purity, the characteristics of the manufactured element can be improved.

In the present embodiment, by heating the purification unit and supplying the carrier gas with a reduced temperature difference from the purification unit, it is possible to prevent temperature reduction and heat non-uniformity in the purification unit due to the carrier gas. Further, by flowing the heated carrier gas into the purification unit, the low temperature region in the enlarged purification unit can be heated and the temperature in the purification unit can be made uniform. Further, since the temperature gradient in the refined part becomes more gradual and continuous due to the heated carrier gas, the impurity and the target substance can be separated with a sufficient distance. Therefore, highly accurate fractionation can be performed and a higher-purity substance can be obtained.

Therefore, by using the purification apparatus and the purification method of this embodiment, a higher-purity substance can be purified with high yield and high productivity.

(Embodiment 4)
In this embodiment, an example of a purification device and a purification method for purifying a higher-purity substance with high yield and high productivity will be described with reference to FIGS. In the refining apparatus and refining method of the second embodiment, the gas temperature adjusting means is an example to be described in detail, and the same function and material may be used for the portion having the same function as that of the second embodiment. The repeated explanation is omitted.

FIG. 4A is a block diagram schematically showing the purification apparatus of the present invention, and FIG. 4B is a cross-sectional view.

The purification apparatus 140 of the present embodiment includes a gas supply unit 142a and a gas discharge unit 142b, a purification unit 142 for purifying and recovering a target substance by vaporizing a substance as a sample, and a gas supply unit to the purification unit 142 A gas supply unit 141 for supplying a gas serving as a carrier gas from 142a, a gas discharge unit 143 for discharging the carrier gas from a gas discharge unit 142b of the purification unit 142, a purification unit temperature adjusting unit for vaporizing and purifying the sample, and The gas temperature adjusting means 144 that also adjusts the temperature of the gas supplied from the gas supplying means 141 by heating is provided. By introducing the carrier gas from the gas supply means 141, the vaporized sample can be diffused smoothly. In this embodiment, when the gas is exhausted from the purifying unit 112, an example is shown in which the gas discharging unit 143 is used to discharge the gas, but the gas discharging unit 143 is not necessarily used.

The purification apparatus 140 according to the present embodiment includes a purification unit temperature adjusting unit that heats to purify a substance, and heating in the gas temperature adjusting unit 144 that heats the carrier gas supplied from the gas supply unit 141 to the purification unit 142. The temperature adjustment means 145 is used in common. As described above, when the heating in the temperature adjusting means is used in common for the purification unit and the gas, the apparatus is simplified, so that the size can be reduced, the space can be saved, and the cost can be reduced. Moreover, since the refinement | purification part and the gas supplied are heated and adjusted to substantially the same temperature, even if it does not set temperature separately, the temperature of a refinement | purification part can be equalized.

As shown in FIG. 4B, the temperature adjusting unit 145 is provided in the vicinity of the purifying unit 142, and the purifying unit 142 is given a temperature gradient by the temperature adjusting unit 145. Specifically, the purification unit 142 is provided with a temperature gradient so that at least the target substance can be isolated, purified, and recovered, such as a temperature range where the sample is vaporized and a temperature range where the target substance is precipitated or condensed.

The refining unit 142 and the temperature adjusting means 145 may be in contact with each other, may be close to each other, or may be in an integrated state. Similarly, the purification unit 142 and the gas supply unit 141 may be in contact with each other, may be close to each other, or may be integrated. “Adjacent” refers to a state in which the space (space) is provided to some extent.

When a metal tube such as tungsten or tantalum is used as the purification unit 142, voltage can be applied to the metal tube and the metal tube can be heated, so that it can be used as the temperature adjusting means 145.

In the present embodiment, in the purification unit 142 for purifying the substance, a part of the gas supplied from the gas supply unit 141 is heated by the temperature adjustment unit 145 before being supplied to the purification unit 142, and the gas temperature adjustment unit 144 A gas adjusted to a high temperature is supplied to the purification unit 142 as a carrier gas. The temperature difference between the temperature of the carrier gas and the temperature of the purifying unit 142 can be reduced by adjusting the temperature of the gas that is supplied and supplied with the preheated gas.

A method for supplying the carrier gas supplied from the gas supply unit 141 to the purification unit 142 will be described in more detail with reference to FIG. In FIG. 4B, the gas supplied from the gas supply means 141 is supplied by opening and closing cocks 149a and 149b that control the supply amount. FIG. 4B shows an example in which the gas is supplied from the two supply ports from the gas supply means 141, but there may be only one supply port, and the supply pipe branches to allow the gas to flow through a plurality of paths. It can also be transported.

FIG. 4C shows an example in which a plurality of gas supply means are provided and gas is supplied from each gas supply means through a supply pipe. In FIG. 4C, the second gas is supplied from the gas supply means 141a through the cock 149a, and the first gas is supplied from the gas supply means 141b through the cock 149b. The gases supplied by the gas supply unit 141a and the gas supply unit 141b may be different materials or the same material. In the same case, it is preferable to use one gas supply unit 141a and one gas supply unit 141b as shown in FIG. 4B because the specification of the apparatus can be simplified.

The gas supplied through the cock 149b of the gas supply means 141 in the gas temperature adjusting means 144 is heated by the heating unit of the temperature adjusting means 145 through the supply pipe 152, and becomes a high temperature first gas. 153. On the other hand, since the gas supplied through the cock 149a of the gas supply means 141 is not heated, it is a second gas having a temperature lower than that of the first gas. The first gas and the second gas having different temperatures are mixed and adjusted to a temperature suitable for supplying to the purification unit. A thermometer for measuring the temperature of the gas for monitoring the temperature may be provided in the supply pipe 154. The temperature-adjusted gas is supplied to the purification unit 142 through the supply pipe 154. In this way, by using a plurality of gases having different temperatures, it is possible to accurately control the temperature of the supplied gas. Further, since the respective flow rates can be appropriately controlled by the cocks 149a and 149b, the temperature control of the carrier gas can be performed more precisely. For example, the temperature of the carrier gas can be controlled appropriately in response to a temperature change of the purification unit during purification.

In the present embodiment, the carrier gas that has been heated to reduce the temperature difference from the purification unit is supplied to the purification unit 142, thereby preventing temperature decrease and heat non-uniformity in the purification unit 142 due to the carrier gas. it can. In addition, by flowing the heated carrier gas into the purification unit 142, the low temperature region in the purification unit 142 that has been enlarged can be heated, and the temperature in the purification unit 142 can be made uniform. Further, since the temperature gradient in the purification unit 142 becomes more moderate and continuous due to the heated carrier gas, the impurity and the target substance can be separated with a sufficient distance. Therefore, highly accurate fractionation can be performed and a higher-purity substance can be obtained.

In the above configuration, the gas supplied to the purification unit used as the carrier gas is an inert gas (nitrogen (N ₂ ), argon (Ar), helium (He), neon (Ne), krypton (Kr), xenon (Xe )) Can be used. Moreover, what is necessary is just to use a pump etc. as a discharge means.

The carrier gas introduced into the purification unit from the gas supply means may be other than an inert gas, but the inert gas is preferred because it can suppress oxidation, decomposition, etc. of the sample and the target substance. Of course, a gas that reacts with the sample or the target substance existing in the purification section must not be used.

Moreover, the purification of the substance can be performed under normal pressure, reduced pressure, or vacuum, and the pressure of the purification unit is controlled by a pressure gauge (vacuum gauge), and the purification unit 142 is operated with a pump or the like used as the gas discharge means 143. What is necessary is just to exhaust the inside through the exhaust pipe 155. FIG. Further, the gas discharge means 143 is not always necessary and may not be used under normal pressure.

What is necessary is just to connect a gas exhausting means and a refinement | purification part using piping etc. Further, a cooling trap using liquid nitrogen or the like may be provided between the purification unit and the gas discharge means. When the inside of the purification unit is depressurized by a vacuum evacuation means to be in a vacuum state, the temperature at which the sample is vaporized can be lowered. That is, when the purification unit is depressurized using the gas discharging means, the sublimation or evaporation temperature of the sample is lowered, and it is possible to vaporize a sample that does not vaporize under atmospheric pressure.

As the temperature adjusting means 145, a heater, a hot plate, or the like may be used, and it may be provided in the vicinity of the purification unit 142 (for example, in the vicinity of a purification tube that vaporizes the sample). 2 shows the case where only one temperature adjusting means 145 is provided in the vicinity of the purification unit 142, the present invention is not limited to this, and a plurality of temperature adjusting means 145 may be provided. The installation location and the number of the temperature adjusting means 145 can be changed as appropriate. Further, in order to keep the temperature gradient applied to the purifying unit 142 constant, a heat insulating unit, a protective cover that surrounds the supply pipes 153 and 154 through which the gas heated by the purifying unit 142 and the gas temperature adjusting unit 144 passes, etc. It is preferable to provide it.

When the temperature of the purification unit 142 is adjusted, it is necessary to set the temperature region such as the temperature at which the sample is vaporized and the temperature at which the target substance is precipitated or condensed to an optimum temperature. This may be set by examining the decomposition point, sublimation point or boiling point of the target substance.

The purification unit 142 is preferably configured by connecting two or more purification tubes. The number of purification tubes arranged in the purification unit 142 can be changed as appropriate. Specifically, it preferably includes two or more purification tubes, including a first purification tube for arranging the sample and a second purification tube for collecting the target substance that has been purified and deposited or condensed. If you do. The basic structure of the purification tube is a hollow tube. The purification tube is provided with an opening at least at the end of the adjacent purification tube so that the vaporized sample (including the target substance and impurities) can pass through. As the purification tube, it is preferable to use a hollow tube made of glass, quartz or the like. In addition, the present invention is not limited to this, and any material that does not react with the sample, the target substance, and impurities, and that can withstand the operating temperature without being mixed into the target substance when the target substance is recovered may be used. In the case of purification at normal pressure, if the purification unit 142 is sealed and heated, the pressure in the tube may increase, which is extremely dangerous. Therefore, either end must be open. Therefore, when using this refinement | purification apparatus by a normal pressure, you have to provide the opening (gas discharge part 142b) at least one place in the refinement | purification part 142 which communicates with the external environment.

Next, the refining section 142 shown in FIG. 4 is provided with a fixing means for fixing between purification steps, and at least a means capable of holding and fixing the state where the purification tubes are arranged adjacent to each other may be used. Preferably, the purification unit 142 may be a means that can be held and fixed so as to be horizontal in the long axis direction. As a fixing means, each purification tube included in the purification unit 142 may be fixed by a clamp or the like, or the purification tube may be arranged on a horizontal base. Moreover, you may arrange | position in pipes, such as glass which has a pipe inner diameter larger than the pipe outer diameter of a refinement | purification pipe | tube.

Further, the purification method in this embodiment can be used for substances such as inorganic compound materials, organic compound materials, or mixed materials of inorganic compounds and organic compounds, and is particularly effective for organic compound materials.

The substance purified in this embodiment can be used for various elements such as a light-emitting element using an organic thin film transistor or an organic electroluminescence element as an example. Since the substance is purified to a high purity, the characteristics of the manufactured element can be improved.

In the present embodiment, by heating the purification unit and supplying the carrier gas with a reduced temperature difference from the purification unit, it is possible to prevent temperature reduction and heat non-uniformity in the purification unit due to the carrier gas. Further, by flowing the heated carrier gas into the purification unit, the low temperature region in the enlarged purification unit can be heated and the temperature in the purification unit can be made uniform. Further, since the temperature gradient in the refined part becomes more gradual and continuous due to the heated carrier gas, the impurity and the target substance can be separated with a sufficient distance. Therefore, highly accurate fractionation can be performed and a higher-purity substance can be obtained.

Therefore, by using the purification apparatus and the purification method of this embodiment, a higher-purity substance can be purified with high yield and high productivity.

(Embodiment 5)
In this embodiment, an example of a purification apparatus and a purification method for purifying a higher-purity substance with high yield and high productivity will be described with reference to FIGS. In the purification apparatus and the purification method of the second and fourth embodiments, it is an example for explaining the gas temperature adjusting means in detail, and the same material and method are used for the parts having the same functions as those of the second and fourth embodiments. The repeated explanation is omitted. In particular, a sublimation purification method in which a target substance and impurities are precipitated as a solid using a solid sample will be described.

5 and 6 are cross-sectional views schematically showing the purification apparatus of the present invention.

The purification apparatus of this embodiment includes a gas supply unit 202a and a gas discharge unit 202b, a purification unit 202 for purifying and recovering a target substance by vaporizing a substance as a sample, and a gas supply unit 202a to the purification unit 202. A gas supply unit 201 for supplying a gas that becomes a carrier gas, a gas discharge unit 203 for discharging the carrier gas from the gas discharge unit 202b of the purification unit 202, a purification unit temperature adjusting unit for vaporizing and purifying the sample, and There is provided a temperature adjusting means 205 that also serves as gas heating in the gas temperature adjusting means for adjusting the temperature of the gas supplied from the gas supply means 201 by heating. By introducing the carrier gas from the gas supply means 201, the vaporized sample can be diffused smoothly. In the present embodiment, when gas is exhausted from the purification unit 202, an example is shown in which gas is discharged from the gas discharge unit 202b using the gas discharge unit 203. However, the gas discharge unit 203 is not necessarily used.

In the present embodiment, the supply pipe 210 (210a, 210b) is provided so that the gas supplied from the gas supply means 201 wraps around the outer periphery of the temperature adjustment means 205 provided so as to surround a part of the periphery of the purification unit 202. Is provided. The gas passing through the supply pipe 210b is heated by the temperature adjusting means 205, and can be supplied to the purification unit 202 through the supply pipe 210a as a gas heated to a high temperature.

The purification apparatus according to the present embodiment uses heating in a purification unit temperature adjusting unit that heats to purify a substance and a gas temperature adjusting unit that heats a carrier gas supplied from the gas supply unit 201 to the purification unit 202. This is performed in common using the adjusting means 205. As described above, when the heating in the temperature adjusting means is used in common for the purification unit and the gas, the apparatus is simplified, so that the size can be reduced, the space can be saved, and the cost can be reduced. Moreover, since the refinement | purification part and the gas supplied are heated and adjusted to substantially the same temperature, even if it does not set temperature separately, the temperature of a refinement | purification part can be equalized.

As shown in FIG. 5, the temperature adjusting unit 205 is provided close to the purifying unit 202, and the purifying unit 202 is given a temperature gradient by the temperature adjusting unit 205. Specifically, the purification unit 202 is provided with a temperature gradient so that at least the target substance can be isolated, purified, and recovered, such as a temperature range where the sample vaporizes and a temperature range where the target substance precipitates or condenses.

The refining unit 202 and the temperature adjusting means 205 may be in contact with each other, may be close to each other, or may be in an integrated state. Similarly, the purification unit 202 and the gas supply unit 201 may be in contact with each other, may be close to each other, or may be in an integrated state. “Adjacent” refers to a state in which the space (space) is provided to some extent.

In the case where a metal tube such as tungsten or tantalum is used as the purifying unit 202, a voltage can be applied to the metal tube and the metal tube can be heated.

In the present embodiment, in the purification unit 202 for purifying the substance, the gas that has been heated by the temperature adjustment unit 205 and adjusted to a high temperature before supplying a part of the gas supplied from the gas supply unit 201 to the purification unit 202. Is supplied to the purification unit 202 as a carrier gas. The temperature difference between the temperature of the carrier gas and the temperature of the purification unit 202 can be reduced by adjusting the temperature of the gas that is supplied and supplied with the preheated gas.

The method for supplying the carrier gas supplied from the gas supply means 201 to the purification unit 202 will be described in more detail with reference to FIG. In FIG. 5, the gas supplied from the gas supply means 201 is supplied by opening and closing cocks 211a and 211b that control the supply amount. FIG. 5 shows an example in which the gas is supplied from the gas supply means 201 through one supply port, and the supply pipe branches to convey the gas through a plurality of paths, but there may be a plurality of supply ports.

FIG. 6 shows an example in which a plurality of gas supply means are provided and gas is supplied from each gas supply means through a supply pipe. In FIG. 6, the second gas is supplied from the gas supply means 201a through the cock 211a, and the first gas is supplied from the gas supply means 201b through the cock 211b. The gases supplied by the gas supply unit 201a and the gas supply unit 201b may be different materials or the same material. In the same case, it is preferable to use one gas supply unit 201a and one gas supply unit 201b as shown in FIG. 5 because the specification of the apparatus can be simplified.

The gas supplied through the cock 211b of the gas supply means 201 is heated by the heating unit of the temperature adjusting means 205 through the supply pipe 210, and is supplied to the supply pipe as a high-temperature first gas. On the other hand, since the gas supplied through the cock 211a of the gas supply means 201 is not heated, it is a second gas having a temperature lower than that of the first gas. The first gas and the second gas having different temperatures are mixed and adjusted to a temperature suitable for supplying to the purification unit. A thermometer 212 for measuring the temperature of the gas for monitoring the temperature may be provided in the supply pipe. The temperature-adjusted gas is supplied to the purification unit 202 through the supply pipe. In this way, by using a plurality of gases having different temperatures, it is possible to accurately control the temperature of the supplied gas. Further, since the respective flow rates can be appropriately controlled by the cocks 211a and 211b, the temperature control of the carrier gas can be performed more precisely. For example, the temperature of the carrier gas can be controlled appropriately in response to a temperature change of the purification unit during purification.

In the present embodiment, the carrier gas that has been heated to reduce the temperature difference from the purification unit is supplied to the purification unit 202, thereby preventing temperature drop and heat non-uniformity in the purification unit 202 due to the carrier gas. it can. Further, by flowing the heated carrier gas into the purification unit 202, the low-temperature region in the enlarged purification unit 202 can be heated and the temperature in the purification unit 202 can be made uniform. Further, since the temperature gradient in the purification unit 202 becomes more gradual and continuous due to the heated carrier gas, the impurity and the target substance can be separated with a sufficient distance. Therefore, highly accurate fractionation can be performed and a higher-purity substance can be obtained.

In the above configuration, the gas supplied to the purification unit used as the carrier gas is an inert gas (nitrogen (N ₂ ), argon (Ar), helium (He), neon (Ne), krypton (Kr), xenon (Xe )) Can be used. Moreover, what is necessary is just to use a pump etc. as a discharge means.

The carrier gas introduced into the purification unit from the gas supply means may be other than an inert gas, but the inert gas is preferred because it can suppress oxidation, decomposition, etc. of the sample and the target substance. Of course, a gas that reacts with the sample or the target substance existing in the purification section must not be used.

Moreover, the purification of the substance can be performed under normal pressure, reduced pressure, or vacuum, and the pressure of the purification unit is controlled by a pressure gauge (vacuum gauge), and the purification unit 202 is controlled by a pump or the like used as the gas discharge means 203. The inside may be exhausted through the discharge pipe 215. Further, the gas discharge means 203 is not always necessary and may be not used under normal pressure.

What is necessary is just to connect a gas exhausting means and a refinement | purification part using piping etc. Further, as shown in FIG. 6, a cooling trap using liquid nitrogen or the like may be provided between the purification unit and the gas discharging means. When the inside of the purification unit is depressurized by a vacuum evacuation means to be in a vacuum state, the temperature at which the sample is vaporized can be lowered. That is, when the purification unit is depressurized using the gas discharging means, the sublimation or evaporation temperature of the sample is lowered, and it is possible to vaporize a sample that does not vaporize under atmospheric pressure. When controlling the pressure in the refinement | purification part 202, it is good to provide the vacuum gauge 257 as shown in FIG. 6, and you may provide the cold trap part 258. FIG.

As the temperature control means 205, a heater, a hot plate, or the like may be used, and it may be provided in the vicinity of the purification unit 202 (for example, in the vicinity of a purification tube for vaporizing a sample). 5 and 6 show the case where only one temperature adjusting means 205 is provided close to the purification unit 202, the present invention is not limited to this, and a plurality of temperature adjusting means 205 may be provided. The installation location and the number of the temperature adjusting means 205 can be changed as appropriate. Further, in order to keep the temperature gradient applied to the purification unit 202 constant, a heat insulating unit, a protective cover surrounding the supply pipes 210a and 210b through which the gas heated by the purification unit 202 and the temperature adjustment unit 205 passes, and the like are provided. Is preferred.

When the temperature of the purification unit 202 is adjusted, it is necessary to set the temperature region such as the temperature at which the sample is vaporized and the temperature at which the target substance is precipitated or condensed to an optimum temperature. This may be set by examining the decomposition point, sublimation point or boiling point of the target substance.

The purification unit 202 is preferably configured by connecting two or more purification tubes. The number of purification tubes arranged in the purification unit 202 can be changed as appropriate. Specifically, it preferably includes two or more purification tubes, including a first purification tube for arranging the sample and a second purification tube for collecting the target substance that has been purified and deposited or condensed. If you do. The basic structure of the purification tube is a hollow tube. The purification tube is provided with an opening at least at the end of the adjacent purification tube so that the vaporized sample (including the target substance and impurities) can pass through. As the purification tube, it is preferable to use a hollow tube made of glass, quartz or the like. In addition, the present invention is not limited to this, and any material that does not react with the sample, the target substance, and impurities, and that can withstand the operating temperature without being mixed into the target substance when the target substance is recovered may be used. In the case of purification at normal pressure, if the purification unit 202 is sealed and heated, the pressure in the pipe may increase, which is extremely dangerous. Therefore, either end must be open. Therefore, when using this refinement | purification apparatus at a normal pressure, you have to provide the opening (gas discharge part 202b) at least one place in the refinement | purification part 202 which communicates with the external environment.

Next, the refining unit 202 shown in FIGS. 5 and 6 is provided with a fixing means for fixing between purification steps, and at least a means capable of holding and fixing the state where the purification tubes are arranged adjacent to each other may be used. Preferably, the purification unit 202 may be a means that can be held and fixed so as to be horizontal in the major axis direction. As the fixing means, each purification tube included in the purification unit 202 may be fixed by a clamp or the like, or the purification tube may be arranged on a horizontal base. Moreover, you may arrange | position in pipes, such as glass which has a pipe inner diameter larger than the pipe outer diameter of a refinement | purification pipe | tube.

Further, the purification method in this embodiment can be used for substances such as inorganic compound materials, organic compound materials, or mixed materials of inorganic compounds and organic compounds, and is particularly effective for organic compound materials.

The substance purified in this embodiment can be used for various elements such as a light-emitting element using an organic thin film transistor or an organic electroluminescence element as an example. Since the substance is purified to a high purity, the characteristics of the manufactured element can be improved.

In the present embodiment, by heating the purification unit and supplying the carrier gas with a reduced temperature difference from the purification unit, it is possible to prevent temperature reduction and heat non-uniformity in the purification unit due to the carrier gas. Further, by flowing the heated carrier gas into the purification unit, the low temperature region in the enlarged purification unit can be heated and the temperature in the purification unit can be made uniform. Further, since the temperature gradient in the refined part becomes more gradual and continuous due to the heated carrier gas, the impurity and the target substance can be separated with a sufficient distance. Therefore, highly accurate fractionation can be performed and a higher-purity substance can be obtained.

Therefore, by using the purification apparatus and the purification method of this embodiment, a higher-purity substance can be purified with high yield and high productivity.

It is the block diagram and sectional drawing which showed the refinement | purification apparatus of this invention. It is the block diagram and sectional drawing which showed the refinement | purification apparatus of this invention. It is the block diagram and sectional drawing which showed the refinement | purification apparatus of this invention. It is the block diagram and sectional drawing which showed the refinement | purification apparatus of this invention. It is sectional drawing which showed the refinement | purification apparatus of this invention. It is sectional drawing which showed the refinement | purification apparatus of this invention.

Claims (3)

A purification unit for vaporizing and purifying the substance;
A temperature adjusting means provided in the refining unit, and providing a temperature gradient to the refining unit;
Gas supply means provided at one end of the purification unit;
A gas discharge unit provided at the other end of the purification unit ;
A gas supply pipe for supplying the gas from the gas supply means to the purification unit ,
The gas supply pipe has a first supply pipe and a second supply pipe,
The temperature adjusting means is provided so as to surround a part of the purification unit,
The second supply pipe is provided to wrap around the temperature adjusting means,
The gas that has passed through the second supply pipe is supplied to the purification section through the first supply pipe . A purification unit for vaporizing and purifying the substance;
A temperature adjusting means provided in the refining unit, and providing a temperature gradient to the refining unit;
Gas supply means provided at one end of the purification unit;
A gas discharge unit provided at the other end of the purification unit ;
A gas supply pipe for supplying the gas from the gas supply means to the purification unit ,
The gas supply pipe has a first supply pipe and a second supply pipe,
The temperature adjusting means is provided so as to surround a part of the purification unit,
The second supply pipe is provided to wrap around the temperature adjusting means ,
The first gas and the second gas are supplied from the gas supply means to the purification unit,
The first gas can pass through the second supply pipe;
The first gas that has passed through the second supply pipe is supplied to the purification unit via the first supply pipe,
The purifying apparatus, wherein the first gas is heated by the temperature adjusting means. In claim 2 ,
The temperature of said 2nd gas is lower than the temperature of said 1st gas, The refinement | purification apparatus characterized by the above-mentioned.

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