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WO2002053250A1 - Procede et dispositif de purification et distillation pour materiaux organiques a point de fusion eleve - Google Patents

Procede et dispositif de purification et distillation pour materiaux organiques a point de fusion eleve Download PDF

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Publication number
WO2002053250A1
WO2002053250A1 PCT/JP2001/011191 JP0111191W WO02053250A1 WO 2002053250 A1 WO2002053250 A1 WO 2002053250A1 JP 0111191 W JP0111191 W JP 0111191W WO 02053250 A1 WO02053250 A1 WO 02053250A1
Authority
WO
WIPO (PCT)
Prior art keywords
temperature
collecting
section
distillation
purification
Prior art date
Application number
PCT/JP2001/011191
Other languages
English (en)
Japanese (ja)
Inventor
Shinji Matsuo
Kazuo Ishii
Hiroshi Miyazaki
Original Assignee
Nippon Steel Chemical Co., Ltd.
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nippon Steel Chemical Co., Ltd. filed Critical Nippon Steel Chemical Co., Ltd.
Publication of WO2002053250A1 publication Critical patent/WO2002053250A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/0011—Heating features
    • B01D1/0017—Use of electrical or wave energy
    • B01D1/0023—Induction heating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D1/00—Evaporating
    • B01D1/30—Accessories for evaporators ; Constructional details thereof
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
    • C07C209/82—Purification; Separation; Stabilisation; Use of additives
    • C07C209/84—Purification

Definitions

  • the present invention relates to a method and an apparatus for purifying a high melting point organic material by distillation.
  • BACKGROUND ART Generally, techniques such as recrystallization, adsorption separation, distillation, and sublimation are used to purify organic materials.
  • Purification using recrystallization is a purification method that uses the difference in solubility of substances depending on the temperature.However, it is difficult to select an available solvent, the solubility difference due to temperature is small, and even if there is a difference in solubility, the solubility itself is low. There may be problems such as requiring a large amount of solvent to purify a small and specified amount.
  • an object of the present invention is to heat a trace amount to a large amount of a feedstock uniformly and in a short time, and to control the heating temperature and the collection temperature with high precision, thereby making it possible to purify a general method. It is an object of the present invention to provide a method and an apparatus for efficiently distilling and refining a high melting point organic material which is difficult to perform.
  • the present invention has an evaporating section for melting and evaporating the high-melting point organic material and a collecting section for condensing and collecting the vaporized gas, and the temperature of the collecting section is substantially stepwise toward the downstream side.
  • At least a part of the evaporator and the collector is made of a material that can be heated by electromagnetic induction. It is a distillation purification device composed of a material that is inert to the organic material having a melting point.
  • a material inert to a high melting point organic material in a molten state a material selected from metals, glass, ceramics, and fluororesins is preferably exemplified. It is also advantageous to provide one or more weirs in the collection area.
  • the present invention has a heating unit and a collecting unit in which at least one layer is made of a metal material, and at least a part of the outer periphery thereof has an induction coil for generating heat by an electromagnetic induction method.
  • This is a distillation purification device in which the collection section is provided with a temperature gradient such that the temperature decreases substantially stepwise or continuously toward the downstream side.
  • the present invention provides a distillation and purification apparatus in which a high-melting-point organic material is charged into an evaporator, heated, melted and evaporated, and the vaporized gas is collected in a collector having a condensing zone maintained in a predetermined temperature range.
  • This is a distillation purification method for recovering purified organic material from the zone after introduction.
  • the organic material to be purified in the present invention is not particularly limited, it has a high melting point, which is difficult to purify by a general method, and is particularly effective for a crystalline solid material in which a crystal takes in a solvent or the like to become a single crystal. Yes, for example, it is effective for solid materials such as electronic materials and optical materials, in which trace impurities or differences in crystal form or deformation often have a large effect. Examples of such a material include an electroluminescent device (EL) material, a semiconductor device material, and the like, which are suitable for an organic EL device material.
  • the electromagnetic induction heating device only needs to generate heat by passing a low-frequency AC current through a coil disposed around a conductive metal material. The frequency of the current is generally 50 to 500 Hz, and a commercial frequency can be used.
  • the heating unit and the collection unit may be continuous or connected in the middle.
  • the heating unit and the collecting unit are preferably cylindrical, but the diameter and the cross-sectional shape may be different in the middle. According to the direction of flow of the organic material to be purified, it has a heating section on the upstream side and a collecting section on the downstream side. At least a part of the heating unit and the collecting unit is made of a conductive metal material so that electromagnetic induction heating can be performed, and a coil is arranged around the conductive metal material.
  • FIG. 1 is a cross-sectional view showing an example of an apparatus for carrying out the purification method of the present invention, which comprises a cylindrical sublimation section A, a collection section B, and a collection section C, each of which is connected in series.
  • FIG. 2 is a cross-sectional view showing an example of a conventional purification device.
  • BEST MODE FOR CARRYING OUT THE INVENTION FIG. 1 is a cross-sectional view showing an example of an apparatus for purifying an organic substance having a high melting point according to the present invention. It consists of part A, collection part B and collection part C.
  • Heating section A has a heating chamber inside, and generates heat by induction current.
  • a cylindrical member 1 made of a metallic material, an induction coil 6 surrounding the outer periphery of the cylindrical member, a heat transfer device 4 and a temperature controller 8.
  • the induction coil 6 is connected to an AC power supply, and the power supply is controlled by a temperature controller 8 connected to the thermocouple 4.
  • the shape of the cylindrical body 1 is not particularly limited, but when it is installed horizontally, it has a semi-cylindrical shape such that the cylinder is divided in half in a length direction, and a flat surface is used as a lower surface. This is preferable because a solid material as a raw material can be easily charged and installed at a predetermined position.
  • the cylindrical body 1 is composed of one layer of metal material, or composed of two or more layers of metal material, it is composed of at least one layer of metal material and another nonmetallic material. No problem. However, at least one of the layers must be made of a metal material that generates heat by induced current, and is preferably a magnetic material.
  • the solid material to be purified may be continuously charged in the form of powder or the like in the heating chamber, but it is convenient to load the material on a boat or the like intermittently and intermittently. If the solid material is easily degraded by heat, it can be charged continuously or in small quantities intermittently.
  • Heating is performed by supplying power, but the amount of power supply is controlled so as to reach the purification temperature in as short a time as possible. Since reducing the heat capacity is also effective for increasing the heating rate, it is advantageous not to increase the diameter of the tubular body 1 or increase the wall thickness more than necessary.
  • a collecting unit that keeps the temperature lower than that is provided.
  • an intermediate zone maintained at an intermediate temperature can be provided between the heating unit A and the collection unit as needed.
  • the trap preferably has a plurality of zones, and at least one zone is capable of induction heating.
  • the collecting portion B is composed of a cylindrical body 2 made of a metallic material, an induction coil 7 surrounding the outer periphery thereof, a thermocouple 5, and a temperature controller 9, and is capable of induction heating.
  • the heating structure of the collecting section B the same structure as that of the heating section A can be applied.However, when the material to be collected is in a liquid state, a weir along an appropriate temperature distribution is provided and a predetermined temperature is provided. It is also effective to classify those condensed in a range.
  • the shape of the weir may be a shape in which the condensed liquid in the predetermined range and the condensed liquid in the other range are not mixed, but a shape such as a ring-shaped partition wall is preferable. It is also effective to provide a withdrawal valve at the bottom. If the material to be collected once becomes liquid and then becomes solid at the collecting part, a valve or the like for withdrawal is unnecessary. Further, a collecting section C is connected downstream of the collecting section B.
  • the collecting portion C is formed of the cylindrical body 3, but the outer periphery thereof may be kept warm, cooled, or come into contact with air. Also, unlike the drawing, it may be placed upstream of the collecting section B.
  • the collection section B which can be induction-heated, may have one stage or two or more stages, but if only one substance is to be collected as the target substance, it is collected. Only the portion to be collected may be capable of induction heating.
  • the collecting section B for induction heating is controlled in temperature so that the substance to be collected is collected with a certain degree of purity, and has a zone of a predetermined length maintained at a certain temperature. You. In other words, there are two or more zones where the temperature is almost constant by induction heating between the heating part and the trapping part, and the temperature is gradually decreased toward the downstream part.
  • the outlet of the most downstream collecting section is connected to the vacuum pump 11 via the trap 10.
  • an organic material which is a raw material
  • an AC power supply is passed from an AC power supply to an induction coil 6, so that a cylindrical body 1 made of a metal material of a heating section A is electromagnetically induced. Heat is generated by heating, and the charge reaches the boiling temperature through melting.
  • the temperature of the cylindrical body 1 is controlled by measuring the temperature of the heating section A with the thermocouple 4, turning the AC power on and off with the temperature controller 8, and controlling the inverter by controlling the inverter. Can be held.
  • the target substance and impurities having a low boiling point in the charged raw material melted in the heating section A are transferred to the collecting section B as gas by the suction force of the vacuum pump 11 behind the collecting section C.
  • the gas transferred to the collecting section B is cooled by the cylindrical body 2 maintained at a temperature equal to or lower than the dew point temperature of the target substance and equal to or higher than the dew point temperature of the contained low-boiling impurities, and the inner wall of the cylindrical body 2 Only the target substance is condensed and collected.
  • the heat generation in the trapping section B and its temperature control can be performed in the same manner as in the heating section A. It is desirable that this temperature be higher than the dew point of the impurities and be as low as possible.However, if the impurities contain a large number of impurities and a small amount of impurities can be tolerated, lower the temperature further. It is also possible to set.
  • the temperature is usually collected as a liquid, but if the temperature is lowered sufficiently, it can be recovered as a solid. However, lowering the temperature sufficiently can be disadvantageous in terms of improving purity. It is also advantageous to condense with a liquid, exist as a liquid during operation, and cool down after operation to form a solid, which is then discharged. If the condensation temperature contains impurities that are nearby, It is preferable to collect in the liquid phase, and it is preferable that the collecting section for collecting the target compound has a multistage structure provided with the above-mentioned barrier wall. If there is no such impurity, it may be promptly collected as a solid.
  • the entire tubular metallic material constituting the tubular body 1.2 is made of a metallic material. It is necessary that there be, or to be formed of two or more layers, and one or more layers be made of a metal material, but it is preferable that at least one of the layers is made of a magnetic metal material. Iron is generally used as such a metal magnetic material, but stainless steel can be used from the viewpoint of heat resistance and corrosion resistance.
  • the induction coil 67 and the temperature controllers 8, 9 used for heating the cylindrical bodies 1 and 2 by electromagnetic induction may be those used in a conventionally known electromagnetic induction heating device.
  • the induction coils 6 and 7 be installed so as to surround the outer circumference of the cylindrical bodies 1 and 2 by a predetermined length.
  • the bodies 1 and 2 By causing the bodies 1 and 2 to generate heat, it is possible to uniformly generate heat in a certain zone of the heating section A and the collecting section B. For example, it takes several minutes to raise the temperature from room temperature to 400 ° C.
  • the heating rate is high, about 30 minutes, and the accuracy of temperature control can be increased.
  • the collecting section B only the target substance is agglomerated and captured, and the impurities in the raw material pass through in a gaseous state, and the impurities are agglomerated in the collecting section C directly connected to the collecting section B. , To capture. Therefore, the collecting section C may be cooled to a predetermined temperature, for example, about room temperature, by air cooling or liquid cooling which is usually performed.
  • the step-like shape means that there are a plurality of zones having a substantially constant temperature in the gas flow direction in the refining device, and does not exclude having a zone where the temperature continuously decreases.
  • the length of the zone where the temperature is almost constant is determined from the viewpoint of securing a trapping capacity of a constant composition.
  • a vacuum pump 11 etc. is installed at the end of the collecting section C. It is good to provide.
  • an accompanying gas such as nitrogen gas is supplied from the entrance direction of the heating section A, and the refining speed can be increased by the accompanying gas.
  • the trapping section B traps impurities
  • the trapping section C traps the target substance.
  • the collecting section for collecting the target substance may be a collecting section capable of induction heating, and the collecting section for collecting impurities may not be capable of induction heating.
  • the heating unit A and the collection unit B have two different temperature zones, that is, one collection unit B that generates heat by using an electromagnetic induction heating method and controls the temperature,
  • one collection unit B that generates heat by using an electromagnetic induction heating method and controls the temperature
  • the purification apparatus provided with one collection unit C by the cooling method has been described, the present invention is not limited to this.
  • a trap that adjusts the temperature by generating heat with an electromagnetic induction type that is adjusted to different temperature zones, such as a case where the collecting section B has two different temperature zones such as Bl and B2. There are two or more junctions, a total of three or more different temperatures It may have a collecting section having a degree zone. Also in the case of the above example, by providing a temperature gradient between the heating section A and the collection sections Bl and B2 and the collection section C, the temperature decreases almost stepwise toward the downstream side. In the trapping section having three different temperature zones, each component in the gas can be reduced according to its melting point.
  • the diameter and length of the cylindrical body used in the refining device are determined as appropriate depending on the type and amount of the organic material, but the device of the present invention can process from a small amount to a large amount, and has a boiling point of 300 ° C. As described above, it is useful for organic materials having a melting point of 200 ° C or more. Furthermore, by reducing the pressure of the purification equipment, it is possible to process at low temperature, which is suitable for purification of unstable substances. 'Examples Hereinafter, the present invention will be specifically described based on examples.
  • the temperature of the collecting section B is set at 300 ° C.
  • the outer periphery of the collecting section C is brought into contact with air at room temperature to maintain the room temperature almost, and the inside of the purification device is reduced by the vacuum pump 11. Was reduced to 0.1 Torr.
  • the amount of NPB recovered from the collecting part B was 5.6 g, and its HPLC purity was 99%. After the operation was completed, the temperature of the collecting section B was lowered, and NPB was recovered as a solid.
  • a heating section A was made of a carbon coconut pipe having a length of 300 ram N and a length of 500 ram, and a collecting section B was made of 100 ram.
  • a carbon steel tube having a diameter of 0 mm and a length of 50 ° mm was used, and a stainless steel tube having a length of 100 mm (i) and a length of 500 ram was used for the collecting section C.
  • Heating section A and collection sections B and C were directly connected via a flange.
  • the same NPB 100 g as used in Example 1 was placed in heating section A by placing it on a glass knot having a length of 200 mm, a width of 250 mm, and a height of 2 Omm.
  • the temperature of the collecting section B at 280 ° C, the outer periphery of the collecting section 3 is kept in contact with air at room temperature and maintained at almost room temperature, and the vacuum pump 11
  • the pressure inside the purification device was reduced to 0.2 Torr.
  • the amount of NPB recovered from the collecting part B was 50.7 g, and its HPLC purity was 99%.
  • Example 2 As shown in FIG. 2, 2.0 g of NPB having an HPLC purity of 94% similar to that used in Example 1 was constituted by a glass outer cylinder 13 and a glass inner cylinder collection section 14 shown in FIG.
  • a high-boiling-point, high-melting-point organic material containing impurities is purified by electromagnetic induction heating, and is collected by a collection unit kept at a specific temperature by electromagnetic induction.
  • the purification equipment can handle small to large quantities, and the accuracy of temperature control is high, and the purification time can be shortened, resulting in high productivity of the purification equipment.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • General Induction Heating (AREA)

Abstract

L'invention porte sur un procédé de distillation et de purification de matériaux à point de fusion élevé, et de prévention de la corrosion du dispositif utilisé, de la contamination du distillat et de prévention de la dégénérescence. L'invention porte également sur un dispositif utilisé dans la réalisation de ce procédé. Le dispositif de distillation et purification comprend une section d'évaporation (A) permettant l'évaporation des matériaux organiques à point de fusion élevé après leur fusion, et des sections de récupération (B, C) prévues pour la condensation et la récupération du gaz évaporé, la température de ces sections de récupération diminuant progressivement ou en continu vers le côté aval. Au moins la section d'évaporation et la partie de la section d'évaporation sont formées dans un matériau pouvant être chauffé par induction électromagnétique par une bobine diélectrique, la surface interne du dispositif étant en contact avec des matériaux organiques à point de fusion élevé est constituée d'un matériau qui est inerte par rapport à ces matériaux organiques à point de fusion élevé. La distillation réalisée au moyen du dispositif de distillation et purification permet de récupérer sélectivement seulement la substance voulue dans les sections de récupération maintenues à une température spécifique par induction électromagnétique. On peut ainsi obtenir un produit de haute pureté à rendement élevé.
PCT/JP2001/011191 2000-12-28 2001-12-20 Procede et dispositif de purification et distillation pour materiaux organiques a point de fusion eleve WO2002053250A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2000402301A JP5248721B2 (ja) 2000-12-28 2000-12-28 高融点有機材料の蒸留精製方法及び装置
JP2000-402301 2000-12-28

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016008312A1 (fr) * 2014-07-15 2016-01-21 广东阿格蕾雅光电材料有限公司 Nouvelle méthode de purification de matériau organique solide

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002235077A (ja) * 2001-02-08 2002-08-23 Nippon Steel Chem Co Ltd 有機ｅｌ材料及びそれを用いた有機ｅｌ素子
KR100437762B1 (ko) * 2001-05-22 2004-06-26 엘지전자 주식회사 유기물질의 정제장치
JP4531429B2 (ja) * 2004-03-31 2010-08-25 保土谷化学工業株式会社 電子製品材料の精製方法
US20160193543A1 (en) * 2012-12-18 2016-07-07 Korea Institute Of Industrial Technology Method and apparatus for purifying organic material using ionic liquid
JP2019111507A (ja) * 2017-12-26 2019-07-11 株式会社 エイエルエステクノロジー 精製装置

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JPS6017337A (ja) * 1983-07-08 1985-01-29 Mitsubishi Heavy Ind Ltd タ−ルの採取方法
US5338518A (en) * 1991-07-09 1994-08-16 Institute Francais Du Petrole Distillation-reaction apparatus and its use for carrying out balanced reaction
JPH09103602A (ja) * 1996-08-13 1997-04-22 Seda Giken:Kk 電磁誘導加熱による分離装置及び分離方法
JPH10273741A (ja) * 1997-03-31 1998-10-13 Sukegawa Electric Co Ltd 溶融金属蒸留装置
JP2000093701A (ja) * 1998-09-25 2000-04-04 Nippon Steel Chem Co Ltd 昇華精製方法及び装置

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Publication number Priority date Publication date Assignee Title
JPS6017337A (ja) * 1983-07-08 1985-01-29 Mitsubishi Heavy Ind Ltd タ−ルの採取方法
US5338518A (en) * 1991-07-09 1994-08-16 Institute Francais Du Petrole Distillation-reaction apparatus and its use for carrying out balanced reaction
JPH09103602A (ja) * 1996-08-13 1997-04-22 Seda Giken:Kk 電磁誘導加熱による分離装置及び分離方法
JPH10273741A (ja) * 1997-03-31 1998-10-13 Sukegawa Electric Co Ltd 溶融金属蒸留装置
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Publication number Priority date Publication date Assignee Title
WO2016008312A1 (fr) * 2014-07-15 2016-01-21 广东阿格蕾雅光电材料有限公司 Nouvelle méthode de purification de matériau organique solide

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