JP4354582B2 - Crystal purification apparatus and method - Google Patents

Crystal purification apparatus and method Download PDF

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Publication number
JP4354582B2
JP4354582B2 JP23536299A JP23536299A JP4354582B2 JP 4354582 B2 JP4354582 B2 JP 4354582B2 JP 23536299 A JP23536299 A JP 23536299A JP 23536299 A JP23536299 A JP 23536299A JP 4354582 B2 JP4354582 B2 JP 4354582B2
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Japan
Prior art keywords
crystal
refining
tower
rotating shaft
purified
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JP2001058103A (en
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良一 渡邊
彰洋 伊藤
健太郎 大田原
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Kureha Corp
Kureha Engineering Co Ltd
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Kureha Corp
Kureha Engineering Co Ltd
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Priority to JP23536299A priority Critical patent/JP4354582B2/en
Priority to PCT/JP2000/005610 priority patent/WO2001014290A1/en
Priority to AU2000265984A priority patent/AU2000265984B2/en
Priority to AU6598400A priority patent/AU6598400A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/004—Fractional crystallisation; Fractionating or rectifying columns
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00—Preparation of halogenated hydrocarbons
    • C07C17/38—Separation; Purification; Stabilisation; Use of additives
    • C07C17/392—Separation; Purification; Stabilisation; Use of additives by crystallisation; Purification or separation of the crystals

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Description

【０００１】
【発明の属する技術分野】
本発明は、不純物を含む原料結晶を精製結晶成分の融解液と向流接触せしめることにより、結晶の精製を行なうこととする結晶精製装置及び方法に関する。
【０００２】
【従来の技術】
従来、結晶の精製装置としては種々の形式のものがあるが、結晶成分の融解液を利用して結晶の精製を行う装置として、例えば特公昭47−40621号公報に開示されたものがある。この公知の装置は、添付図面の図３に示されるように、下部に不純物を含む被精製物質としての原料粗結晶を精製塔１１内に供給する手段として、仕込口１２内にスクリューコンベア１３を有し、塔上部に配設された加熱融解装置１４により結晶を融解させ、その融解液と精製塔１１内を上昇してくる結晶と向流接触させながら、精製された結晶を上部の取出口１５から取り出す直立型精製装置を成している。精製塔１１内には回転軸体１６に攪拌翼１７を取り付けた攪拌機１８が設けられ、この攪拌機１８は、上記仕込口１２より供給された結晶を解きほぐしながら上昇させる機能を有している。
【０００３】
このような構成の結晶精製装置により目的結晶成分の融解液を利用して不純物を含む粗結晶を精製するには、原料粗結晶は精製塔１１の仕込口１２より塔内へ供給され、塔内に設けた攪拌機１８により塔頂に向かって揚昇される。その際、攪拌機１８は、結晶が塊のまま上昇したり或いは結晶が攪拌翼１７に付着したりするのを防ぎつつ結晶を解きほぐし精製塔１１内を輸送上昇させる。かくして塔頂に達した結晶は、必要量が融解され還流融解液となって重力によって精製塔１１内を下降し、この融解液で洗浄されながら塔頂に達した結晶は目的とする純度で取出口１５から取り出される。なお、原料結晶に含まれていた不純物は精製塔１１内を下降して濾過装置１９で分離され排出口２０から除去される。
【０００４】
【発明が解決しようとする課題】
しかしながらこの精製装置は、塔上部に加熱融解装置１４を設置しているため、該加熱融解装置１４が上昇してくる結晶より強い圧力を受け、さらにはその圧力の反力によって攪拌機１８への負荷が増大し、その結果、加熱融解装置そして攪拌機が損傷することがあった。
【０００５】
さりとて、このような問題を操作上防ぐためには結晶の処理量を下げざるをえず、生産能力の低下をきたすことになる。また、上記圧力を小さくするために加熱融解装置を小さくすると、伝熱面積が減少してしまうので、加熱融解装置で同じ供給熱量を確保しようとすると、融解液の温度が上昇し、その結果、融解液が変質するという問題を生ずる。
【０００６】
さらに、この種の装置では結晶の上昇量が変動する場合があるが、これに対応することが難しい。すなわち、図３の装置にあっては、装置の制御は、加熱融解装置の温度を加減することにより融解液の温度や量を調整するので、この融解液の温度や量の調整は間接的になされる。したがって、この制御は適正条件下でなされることがきわめて困難となって操業条件が変動してしまい、伝熱係数もその変動を受け、その結果、加熱融解装置で与える熱量も変動して不安定となり、結晶の熱による変質、さらには精製能力の低下を招いていた。
【０００７】
本発明は、かかる事情に鑑み、融解液の温度や量といった条件を直接制御して高品質な製品を安定して高能力で精製できる結晶精製装置及び方法を提供することを目的とする。
【０００８】
【課題を解決するための手段】
本発明に係る結晶精製装置は、縦方向に延びる筒型の精製塔の下部に原料結晶の仕込口を、上部に精製後の結晶を製品として取出すための取出口とを有している。この精製塔内には、原料結晶の攪拌のための攪拌装置が配設されており、該精製塔内での精製結晶成分の降下融解液と上昇原料結晶との向流接触により原料結晶が精製される。
【０００９】
かかる結晶精製装置において、本発明では、精製結晶成分の融解液を外部から精製塔内へ供給する融解液供給手段が該精製塔上部に設けられていることを特徴としている。
【００１０】
このような本発明装置にあっては、精製結晶成分の融解液が外部から精製塔の上部にて該精製塔内へ降下供給され、上昇原料結晶が精製塔内で精製結晶成分の降下融解液と向流接触して精製される。
【００１１】
本発明において、攪拌装置は、原料結晶の攪拌と共に上方への押し上げが可能であることが好ましい。その場合、攪拌装置は、縦方向に延びる回転軸体に取りつけられた攪拌翼を有しているようにすることができる。上記攪拌装置は回転軸体を複数有し、各回転軸体に回転翼が取りつけられている形態とすることができる。その際、複数の回転軸体の少なくとも一つは他の回転軸体と逆方向に回転しているようにすることが可能である。複数の回転軸体に取りつけられた回転翼は、回転軸体の軸線方向から見たときに、回転面同士が一部重なっているならば、攪拌効果が向上する。
【００１２】
さらに、本発明において、仕込口には、原料結晶を精製塔に押し込むことのできる供給装置が接続されているようにすることが望ましく、こうすることにより原料結晶の供給能力の向上が図れる。又、精製塔は下部に濾過装置そしてその下方に不純物排出口が設けられていることが好ましい。
【００１３】
【発明の実施の形態】
以下、添付図面の図１及び図２にもとづき、本発明の実施の形態について説明する。
【００１４】
図において、精製塔１は縦型筒状をなしており、内部に攪拌装置２が配設されている。攪拌装置２は、本実施形態においては、縦に延びる回転軸体２Ａを二本有し、各回転軸体２Ａに複数の攪拌翼２Ｂが取りつけられている。二本の回転軸体２Ａは、同方向に回転してもあるいは逆方向に回転していてもよい。いずれにしても、攪拌翼２Ｂは回転軸体２Ａの回転時に上昇流を形成するような水平面に対しての傾角を有していることが好ましい。二つの回転軸体２Ａに取りつけられた攪拌翼２Ｂは、本実施形態では好ましい形態として図２に見られるように、上方から見たときに両方の攪拌翼２Ｂの回転面が一部重なり合うようになっている。この重なり合う領域にて攪拌能力は向上する。上記精製塔１の内壁面はかかる回転面の円に近接した形をなすことが好ましい。
【００１５】
上記精製塔１の下部には仕込口３が設けられており、ここから原料結晶が供給されるようになっている。この仕込口３には、図示していないが、スクリューコンベア等の供給装置が設けられていて、原料結晶を精製塔１内へ押し込むことが可能となっていることが好ましい。
【００１６】
上記精製塔１の上部には、精製後の結晶を製品として取り出すための取出口４と、精製結晶成分の融解液を外部から精製塔内へ供給するための融解液供給手段５とが設けられている。上記融解液供給手段５は、本実施形態においては、供給管の形態をなしており、温度等の状況が予め正確に判っている融解液が所定量だけ供給されるようになっている。
【００１７】
さらに、上記精製塔１内の下部に濾過装置６が配設されていると共に、底部には不純物排出口７が設けられている。
【００１８】
かかる本実施形態装置においては、原料粗結晶またはスラリー状結晶混合物は仕込口３から精製塔１内部に送り込まれる。このようにして送り込まれた原料結晶は攪拌機２によって攪拌されながら塔上部へ運ばれる。塔上部では融解液供給手段５より結晶成分の融解液が塔外から供給される。この融解液は温度等の状況が正確に把持されており、装置の運転管理上最適な量だけ供給される。この融解液の一部は塔内を下降して、上昇してくる原料結晶と向流接触する。これにより、上昇せる結晶は洗浄され、又、温度上昇による発汗作用により結晶内部の不純物を外に吐き出すことで精製される。このようにして原料結晶が塔上部に達したときには、原料結晶は精製されて高純度の物質になっており、ここでその一部分は取出口４から製品として取り出される。
【００１９】
粗原料結晶に含まれていた低融点不純物は塔内を下降して濾過装置６で結晶と分離されて不純物排出口７から排出される。
【００２０】
本発明は、以上の実施形態に示された具体例に限定されるものではない。融解液供給手段は、図示のような供給管でなくても、多孔板のような、融解液を少量ずつ均等に降らすようなものでもよい。又、精製塔は必ずしも円筒型でなくてもよく、任意の断面形状をとり得るし、あるいは垂立していなくとも多少傾斜していてもよい。
<実施例>
内径508mm、高さ約2600mmの２つの円筒を重ねあわせた図２のごとくの断面形状の精製塔を有する精製装置に、パラジクロルベンゼン92.3％、オルソジクロルベンゼン6.6％、メタジクロルベンゼン1.1％のスラリー状態の混合物を1514kg/Hrで仕込み、降らした融解液を除いて正味1260kg/Hrの純度99.99％以上のパラジクロルベンゼンを得ることができた。この装置と同じ大きさの特公昭47-40621号公報に開示された精製装置では、800kg/Hrが限度であった。
【００２１】
【発明の効果】
本発明は、以上説明したように、従来装置のように加熱融解装置を精製塔上部に配設することがないので、融解装置が上昇結晶からの圧力を受け、そして攪拌機がその反力を受けてそれぞれ損傷する可能性がなくなった。
【００２２】
さらには、温度等の条件が正確に把握されている融解液を外部から所望な適正量だけ供給するので、条件制御が正確にできる。その結果、熱による変質のない高品質な製品を安定して高精製能力のもとに得られる。
【図面の簡単な説明】
【図１】本発明の一実施形態装置の縦断面図である。
【図２】図１装置のII−II断面図である。
【図３】従来装置の縦断面図である。
【符号の説明】
１ 精製塔
２ 攪拌装置
２Ａ 回転軸体
２Ｂ 攪拌翼
３ 仕込口
４ 取出口
５ 融解液供給手段
６ 濾過装置
７ 不純物排出口[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a crystal purification apparatus and method for purifying a crystal by bringing a raw material crystal containing impurities into countercurrent contact with a melt of a purified crystal component.
[0002]
[Prior art]
Conventionally, there are various types of crystal refining apparatuses, but there is an apparatus disclosed in, for example, Japanese Examined Patent Publication No. 47-40621 as an apparatus for purifying crystals using a melt of a crystal component. As shown in FIG. 3 of the accompanying drawings, this known apparatus is provided with a screw conveyor 13 in a charging port 12 as means for supplying raw crystal as a material to be purified containing impurities at the bottom into a purification tower 11. The melting crystal is melted by a heating and melting device 14 provided at the upper part of the tower, and the purified crystal is brought into countercurrent contact with the rising liquid and the crystal rising in the purification tower 11, and the purified crystal is removed from the upper outlet. 15 constitutes an upright purifier. In the refining tower 11, a stirrer 18 having a rotating shaft body 16 and a stirring blade 17 is provided, and this stirrer 18 has a function of lifting the crystal supplied from the charging port 12 while unraveling it.
[0003]
In order to purify a crude crystal containing impurities by using the melt of the target crystal component by the crystal purification apparatus having such a configuration, the raw material crude crystal is supplied into the tower through the charging port 12 of the purification tower 11, It is lifted toward the top of the tower by a stirrer 18 provided in At that time, the stirrer 18 unraveles the crystals and prevents the crystals from adhering to the stirring blades 17 while transporting up the purification tower 11 while preventing the crystals from rising as a lump or adhering to the stirring blades 17. Thus, the crystals that have reached the top of the tower are melted in a necessary amount to become a refluxing melt, descended in the purification tower 11 by gravity, and the crystals that have reached the top of the tower while being washed with this melting liquid are collected with the desired purity. It is taken out from the outlet 15. The impurities contained in the raw material crystals descend in the purification tower 11 and are separated by the filtering device 19 and removed from the outlet 20.
[0004]
[Problems to be solved by the invention]
However, in this refining apparatus, since the heating and melting apparatus 14 is installed in the upper part of the tower, the heating and melting apparatus 14 receives a pressure stronger than the rising crystal, and further, the load on the stirrer 18 is caused by the reaction force of the pressure. As a result, the heating and melting apparatus and the stirrer may be damaged.
[0005]
In the meantime, in order to prevent such a problem in operation, it is necessary to reduce the processing amount of crystals, resulting in a decrease in production capacity. In addition, if the heating and melting apparatus is reduced in order to reduce the pressure, the heat transfer area is reduced, so if the same amount of supplied heat is secured with the heating and melting apparatus, the temperature of the melt rises. This causes the problem that the melt is altered.
[0006]
Furthermore, in this type of apparatus, the amount of rising of the crystal may fluctuate, but it is difficult to cope with this. That is, in the apparatus of FIG. 3, since the control of the apparatus adjusts the temperature and the amount of the melt by adjusting the temperature of the heating and melting apparatus, the adjustment of the temperature and the amount of the melt is indirectly performed. Made. Therefore, this control is extremely difficult to be performed under appropriate conditions, and the operating conditions fluctuate. The heat transfer coefficient is also affected, and as a result, the amount of heat given by the heating and melting apparatus also fluctuates and becomes unstable. As a result, the crystal was altered by heat and the purification ability was lowered.
[0007]
In view of such circumstances, an object of the present invention is to provide a crystal purification apparatus and method that can directly control conditions such as the temperature and amount of a melt to stably purify a high-quality product with high performance.
[0008]
[Means for Solving the Problems]
The crystal refining apparatus according to the present invention has a raw material crystal charging port at the lower part of a cylindrical refining tower extending in the vertical direction, and an outlet for taking out the purified crystal as a product at the upper part. In this purification tower, a stirrer for stirring the raw material crystal is arranged, and the raw material crystal is purified by countercurrent contact between the falling melt of the purified crystal component and the rising raw material crystal in the purification tower. Is done.
[0009]
In such a crystal purification apparatus, the present invention is characterized in that a melt supply means for supplying a melt of the purified crystal component from the outside into the purification tower is provided in the upper part of the purification tower.
[0010]
In such an apparatus of the present invention, the melt of the purified crystal component is supplied from the outside to the purifier tower at the upper part of the purifier tower, and the ascending raw material crystal is the descended melt of the purified crystal component in the purifier tower. And purified in countercurrent contact.
[0011]
In the present invention, it is preferable that the stirring device can be pushed upward together with the stirring of the raw crystal. In that case, the stirring device may have a stirring blade attached to a rotating shaft that extends in the longitudinal direction. The stirring device may have a plurality of rotating shaft bodies, and a rotating blade may be attached to each rotating shaft body. At this time, at least one of the plurality of rotating shaft bodies can be rotated in the opposite direction to the other rotating shaft bodies. If the rotating blades attached to the plurality of rotating shaft bodies are partially overlapped with each other when viewed from the axial direction of the rotating shaft body, the stirring effect is improved.
[0012]
Furthermore, in the present invention, it is desirable that a supply device that can push the raw material crystal into the purification tower is connected to the charging port, whereby the supply ability of the raw material crystal can be improved. The purification tower is preferably provided with a filtration device at the bottom and an impurity discharge port below it.
[0013]
DETAILED DESCRIPTION OF THE INVENTION
Hereinafter, embodiments of the present invention will be described with reference to FIGS. 1 and 2 of the accompanying drawings.
[0014]
In the figure, the purification tower 1 has a vertical cylindrical shape, and a stirrer 2 is disposed therein. In this embodiment, the stirring device 2 has two rotating shaft bodies 2A extending vertically, and a plurality of stirring blades 2B are attached to each rotating shaft body 2A. The two rotating shaft bodies 2A may rotate in the same direction or in opposite directions. In any case, it is preferable that the stirring blade 2B has an inclination angle with respect to a horizontal plane that forms an upward flow when the rotary shaft 2A rotates. The stirring blades 2B attached to the two rotary shaft bodies 2A are, as seen in FIG. 2 as a preferred embodiment in this embodiment, so that the rotation surfaces of both stirring blades 2B partially overlap when viewed from above. It has become. The stirring ability is improved in this overlapping region. The inner wall surface of the purification tower 1 preferably has a shape close to the circle of the rotating surface.
[0015]
A charging port 3 is provided in the lower part of the purification tower 1, from which raw material crystals are supplied. Although not shown, the charging port 3 is preferably provided with a supply device such as a screw conveyor so that the raw material crystals can be pushed into the purification tower 1.
[0016]
In the upper part of the purification tower 1, there are provided an outlet 4 for taking out the purified crystal as a product, and a melt supply means 5 for supplying a melt of the purified crystal component from the outside into the purification tower. ing. In the present embodiment, the melt supply means 5 is in the form of a supply pipe so that a predetermined amount of a melt whose temperature and the like are accurately known in advance is supplied.
[0017]
Further, a filtration device 6 is disposed in the lower part of the purification tower 1, and an impurity discharge port 7 is provided at the bottom.
[0018]
In the apparatus of this embodiment, the raw raw crystal or slurry crystal mixture is fed into the purification tower 1 from the charging port 3. The raw material crystals fed in this way are carried to the upper part of the tower while being stirred by the stirrer 2. In the upper part of the tower, the melt of the crystal component is supplied from the outside of the tower from the melt supply means 5. This melt is accurately grasped in terms of temperature and the like, and is supplied in an amount optimal for operation management of the apparatus. A part of the molten liquid descends in the tower and comes into countercurrent contact with the rising raw material crystals. As a result, the rising crystal is washed and purified by exhaling impurities inside the crystal to the outside by the sweating action caused by the temperature rise. When the raw material crystal reaches the top of the tower in this way, the raw material crystal is refined into a high-purity substance, and a part thereof is taken out from the outlet 4 as a product.
[0019]
The low-melting point impurities contained in the raw material crystals descend in the tower, are separated from the crystals by the filtration device 6, and are discharged from the impurity discharge port 7.
[0020]
The present invention is not limited to the specific examples shown in the above embodiments. The melt supply means may not be a supply pipe as shown in the figure, but may be a perforated plate that uniformly drops the melt little by little. Further, the purification tower does not necessarily have to be a cylindrical shape, and can have an arbitrary cross-sectional shape, or may be slightly inclined even if it does not stand upright.
<Example>
In a refining unit with a refining tower with a cross-sectional shape as shown in Fig. 2 in which two cylinders with an inner diameter of 508 mm and a height of about 2600 mm are stacked, a slurry of paradichlorobenzene 92.3%, orthodichlorobenzene 6.6%, and metadichlorobenzene 1.1% The mixture in the state was charged at 1514 kg / Hr, and excluding the molten solution, paradichlorobenzene having a net of 1260 kg / Hr and a purity of 99.99% or more could be obtained. In the refining apparatus disclosed in Japanese Patent Publication No. 47-40621 having the same size as this apparatus, the limit was 800 kg / Hr.
[0021]
【The invention's effect】
As described above, in the present invention, since the heating and melting apparatus is not provided at the upper part of the purification tower unlike the conventional apparatus, the melting apparatus receives pressure from the rising crystal and the stirrer receives the reaction force. The possibility of damaging each was eliminated.
[0022]
Furthermore, since a desired appropriate amount of melt from which the conditions such as temperature are accurately grasped is supplied from the outside, condition control can be performed accurately. As a result, it is possible to stably obtain a high-quality product that is not deteriorated by heat with high refining ability.
[Brief description of the drawings]
FIG. 1 is a longitudinal sectional view of an apparatus according to an embodiment of the present invention.
2 is a cross-sectional view of the apparatus shown in FIG. 1 taken along the line II-II.
FIG. 3 is a longitudinal sectional view of a conventional device.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1 Purification tower 2 Stirring apparatus 2A Rotating shaft 2B Stirring blade 3 Charge port 4 Outlet 5 Melt supply means 6 Filtration apparatus 7 Impurity discharge port

Claims (9)

縦方向に延びる筒型の精製塔の下部に原料結晶の仕込口と上部に精製後の結晶を製品として取出すための取出口とをそれぞれ設け、原料結晶の攪拌のための攪拌装置を上記精製塔内に配設し、精製塔内での精製結晶成分の降下融解液と上昇原料結晶との向流接触により原料結晶を精製する結晶精製装置において、精製結晶成分の融解液を外部から精製塔内へ供給する融解液供給手段が該精製塔上部に設けられていることを特徴とする結晶精製装置。A raw material crystal charging port is provided at the bottom of a cylindrical refining tower extending in the vertical direction, and an outlet for taking out the purified crystal as a product is provided at the top, respectively. In a crystal refining device that is disposed inside and purifies the raw crystal by countercurrent contact between the descending melt of the purified crystal component and the ascending raw material crystal in the purification tower, the melt of the purified crystal component is externally introduced into the purification tower. A crystal refining apparatus, characterized in that a melt supplying means for supplying to the top of the refining tower is provided. 攪拌装置は、原料結晶の攪拌と共に上方への押し上げが可能であることとする請求項１に記載の結晶精製装置。The crystal purifier according to claim 1, wherein the stirring device can push up the raw material crystal together with stirring. 攪拌装置は、縦方向に延びる回転軸体に取りつけられた攪拌翼を有していることとする請求項１又は請求項２に記載の結晶精製装置。The crystal refining device according to claim 1 or 2, wherein the stirring device has a stirring blade attached to a rotating shaft body extending in the longitudinal direction. 攪拌装置は回転軸体を複数有し、各回転軸体に回転翼が取りつけられていることとする請求項３に記載の結晶精製装置。4. The crystal refining device according to claim 3, wherein the stirring device has a plurality of rotating shaft bodies, and a rotating blade is attached to each rotating shaft body. 複数の回転軸体の少なくとも一つは他の回転軸体と逆方向に回転していることとする請求項４に記載の結晶精製装置。The crystal refining device according to claim 4, wherein at least one of the plurality of rotating shaft bodies rotates in a direction opposite to that of the other rotating shaft bodies. 複数の回転軸体に取りつけられた回転翼は、回転軸体の軸線方向から見たときに、回転面同士が一部重なっていることとする請求項４又は請求項５に記載の結晶精製装置。The crystal refining device according to claim 4 or 5, wherein the rotating blades attached to the plurality of rotating shaft bodies partially overlap each other when viewed from the axial direction of the rotating shaft body. . 仕込口には、原料結晶を精製塔に押し込むことのできる供給装置が接続されていることとする請求項１に記載の結晶精製装置。The crystal purifier according to claim 1, wherein a supply device capable of pushing the raw crystal into the purification tower is connected to the charging port. 精製塔は下部に濾過装置そしてその下方に不純物排出口が設けられていることとする請求項１に記載の結晶精製装置。2. The crystal purification apparatus according to claim 1, wherein the purification tower is provided with a filtration device at the bottom and an impurity discharge port below the filtration device. 縦方向に延びる筒型の精製塔の下部に原料結晶の仕込口と上部に精製後の結晶を製品として取出すための取出口とをそれぞれ設け、原料結晶の攪拌のための攪拌装置を上記精製塔内に配設し、精製塔内で精製結晶成分の降下融解液と上昇原料結晶とを向流接触せしめて原料結晶を精製する結晶精製方法において、精製結晶成分の融解液を外部から精製塔の上部にて該精製塔内へ降下供給することを特徴とする結晶精製方法。A raw material crystal charging port is provided at the bottom of a cylindrical refining tower extending in the vertical direction, and an outlet for taking out the purified crystal as a product is provided at the top, respectively. In the crystal purification method in which the purified crystal component is purified by bringing the purified crystal component descending melt and the ascending raw material crystal into countercurrent contact in the purification tower to purify the raw material crystal, A crystal refining method, characterized in that the lower part is supplied into the refining tower at the top.
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