JPS63209702A - Method for operating crystallizer - Google Patents
Method for operating crystallizerInfo
- Publication number
- JPS63209702A JPS63209702A JP62040199A JP4019987A JPS63209702A JP S63209702 A JPS63209702 A JP S63209702A JP 62040199 A JP62040199 A JP 62040199A JP 4019987 A JP4019987 A JP 4019987A JP S63209702 A JPS63209702 A JP S63209702A
- Authority
- JP
- Japan
- Prior art keywords
- draft tube
- crystal
- outside
- flow
- crystallizer
- Prior art date
- Legal status (The legal status 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 status listed.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims description 9
- 239000013078 crystal Substances 0.000 claims abstract description 50
- 238000003756 stirring Methods 0.000 claims description 13
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 238000002425 crystallisation Methods 0.000 description 7
- 230000008025 crystallization Effects 0.000 description 7
- 239000000243 solution Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- 239000011550 stock solution Substances 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0036—Crystallisation on to a bed of product crystals; Seeding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
Landscapes
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野〕
この発明は肥料、食品、薬品などの種々の有機化学工業
分野および無機化学工業分野において、分離、精製、回
収などのために広く用いられている結晶缶の運転方法に
関するものである。[Detailed Description of the Invention] (Industrial Application Field) This invention is widely used for separation, purification, recovery, etc. in various organic and inorganic chemical industries such as fertilizers, foods, and drugs. This relates to a method of operating a crystal canister.
従来、この種の結晶化装置は一例をあげれば第２図に示
すような構造を有している。すなわち同図において、１
は結晶缶、２は加熱器であり３は遠心分離機である。そ
して結晶缶１には中央部に立設されて、液を循環させる
ドラフトチューブ４、このチューブ４内の下方に設けら
れた撹拌機５、セットリング域（上部から微粒子を含む
溶液を取出す） ６と循環域を分離するバッフルプレー
ト７、分級脚８、蒸発蒸気排出口９などを有している。Conventionally, this type of crystallization apparatus has a structure as shown in FIG. 2, for example. In other words, in the same figure, 1
is a crystallizer, 2 is a heater, and 3 is a centrifuge. The crystal can 1 has a draft tube 4 erected in the center to circulate the liquid, a stirrer 5 provided below the tube 4, and a settling area 6 (for taking out the solution containing fine particles from the top). It has a baffle plate 7 that separates the circulation area and the circulation area, a classification leg 8, an evaporative steam outlet 9, etc.
なお１０は循環ポンプ、１１は取出しポンプ、１２は補
助ポンプ、１３は原液供給管、１４は結晶取出し口、１
５は加熱蒸気供給管、１６は循環管、１７は循環回路、
１８は撹拌翼を示す。又前記ドラフトチューブ４は図示
しないサポートにより結晶缶１の缶壁またはバッフルプ
レート ７に固定されている。In addition, 10 is a circulation pump, 11 is a take-out pump, 12 is an auxiliary pump, 13 is a stock solution supply pipe, 14 is a crystal take-out port, 1
5 is a heating steam supply pipe, 16 is a circulation pipe, 17 is a circulation circuit,
18 indicates a stirring blade. Further, the draft tube 4 is fixed to the can wall of the crystal can 1 or the baffle plate 7 by a support (not shown).
原液は供給管１３から供給され、加熱器２で加熱され、
結晶缶１に送入され蒸発が行われる。The stock solution is supplied from the supply pipe 13 and heated by the heater 2,
It is fed into the crystal canister 1 and evaporated.
缶内の液は撹拌機５の作動によりドラフトチューブ４内
を上昇し、かつその外部を下降し、循環が行われる。蒸
発により過飽和となった溶液は缶内底部に滞溜する結晶
１９またはドラフトチューブ４内を上昇してきた結晶１
９と接触し、晶析が行われて結晶が成長する。The liquid in the can rises in the draft tube 4 by the operation of the stirrer 5 and descends outside the draft tube 4, thereby performing circulation. The solution that has become supersaturated due to evaporation is either crystals 19 that accumulate at the bottom of the can or crystals 1 that have risen in the draft tube 4.
9, crystallization occurs and crystals grow.
成長した結晶は分級脚８から取出される。また微１ｉＩ
ｉｌな結晶は溶液と共にセットリング域６上端から循環
管１６を経て取出されて原液と混合され加熱溶解された
後再び結晶缶に戻される。The grown crystals are taken out from the classification leg 8. Also fine 1iI
The ill crystals are taken out along with the solution from the upper end of the settling area 6 via the circulation pipe 16, mixed with the stock solution, heated and dissolved, and then returned to the crystal can.
かかる結晶缶は、缶内における溶液と結晶の流動が活発
なので、結晶の成長が早く、大粒径の結晶が得やすいと
いう特徴がある反面、比較的大粒径の結晶もドラフトチ
ューブ４内を循環流と共に上昇し缶内を循環するので、
その際結晶が撹拌翼１８に当り結晶が傷つけられる。結
晶が傷つけられると結晶中に不純物や液が巻き込まれる
ため結晶の品質に問題がでる場合がある。Such a crystal can has the characteristics that the solution and crystals flow actively in the can, so the crystals grow quickly and it is easy to obtain crystals with a large grain size. As it rises with the circulation flow and circulates inside the can,
At this time, the crystal hits the stirring blade 18 and is damaged. If the crystal is damaged, impurities or liquid may be drawn into the crystal, which may cause problems with the quality of the crystal.
本発明は従来の結晶缶の運転方法のかかる問題点に鑑み
案出されたもので、結晶の成長が早いにもかかわらず、
結晶に傷がなく優れた品質の結晶を製造できる結晶缶の
運転方法を提供することを目的とする。The present invention was devised in view of the problems with the conventional method of operating a crystallizer, and despite the rapid growth of crystals,
An object of the present invention is to provide a method for operating a crystal can that can produce crystals of excellent quality without scratches on the crystals.
（問題点を解決するための手段）
上記目的を達成するため本発明の結晶缶の運転方法は、
缶内中央部に立設される上下端開放のドラフトチューブ
と、該ドラフトチューブを囲繞して設けられ、循環域と
セットリング域を分離する筒状のバッフルプレートと、
ドラフトチューブ内下方に設けられ、ドラフトチューブ
内側と外側との間を循環する循環流を起す撹拌翼とを備
えた結晶缶を用いて結晶を析出させる結晶缶の運転方法
において、上記撹拌翼により発生する循環流はドラフト
チューブ内側が下降流、ドラフトチューブ外側が上昇流
となっており、且つ撹拌翼の回転数および／またはピッ
チが調節されて、ドラフトチューブ外側の上昇流の流速
は、上昇流により所要大きさ以上の結晶粒が舞い上りド
ラフトチューブ上端を越えて循環する流速より小さくな
っていることを特徴とするものである。(Means for Solving the Problems) In order to achieve the above object, the method of operating a crystallizer according to the present invention is as follows:
a draft tube with open upper and lower ends that stands in the center of the can; a cylindrical baffle plate that surrounds the draft tube and separates a circulation area and a settling area;
In a method of operating a crystallizer in which crystals are precipitated using a crystallizer equipped with a stirring blade which is provided in the lower part of the draft tube and generates a circulating flow between the inside and outside of the draft tube, The circulating flow is a downward flow on the inside of the draft tube and an upward flow on the outside of the draft tube, and the rotation speed and/or pitch of the stirring blades is adjusted so that the velocity of the upward flow on the outside of the draft tube is increased by the upward flow. It is characterized in that crystal grains larger than the required size fly up and the flow velocity is lower than the circulating flow rate beyond the upper end of the draft tube.
以下、本発明の一実施例について図面を参照しつつ説明
する。An embodiment of the present invention will be described below with reference to the drawings.
第１図は本発明の運転方法を具体化した結晶化装置のフ
ローシートである。第１図において１は結晶缶、２は加
熱器、３は遠心分離機、４はドラフトチューブ、５は撹
拌機、６はセットリング域、 ７はバッフルプレート、
８は分級脚、９は蒸発蒸気排出口、１０は循環ポンプ、
１１は取出しポンプ、１２は補助ポンプ、１３は原液供
給管、１４は結晶取出し口、１５は加熱蒸気供給管、１
６は循環管、１７は循環回路、１８は撹拌翼、１９は結
晶、２０は循環流の流れ方向を示す矢印である。尚第１
図の結晶化装置は第２図に示す結晶化装置と装置的には
ほぼ同じであるので同一のエレメントについては同一の
符号を用いてあり、説明を省略する。FIG. 1 is a flow sheet of a crystallization apparatus embodying the operating method of the present invention. In Figure 1, 1 is a crystallizer, 2 is a heater, 3 is a centrifuge, 4 is a draft tube, 5 is a stirrer, 6 is a settling area, 7 is a baffle plate,
8 is a classification leg, 9 is an evaporative steam outlet, 10 is a circulation pump,
11 is a take-out pump, 12 is an auxiliary pump, 13 is a stock solution supply pipe, 14 is a crystal take-out port, 15 is a heated steam supply pipe, 1
6 is a circulation pipe, 17 is a circulation circuit, 18 is a stirring blade, 19 is a crystal, and 20 is an arrow indicating the flow direction of the circulation flow. Furthermore, the first
Since the crystallization apparatus shown in the figure is almost the same as the crystallization apparatus shown in FIG. 2 in terms of apparatus, the same elements are denoted by the same reference numerals, and the explanation thereof will be omitted.
撹拌翼１８を回転させると、第１図の矢印２０で示すよ
うにドラフトチューブ４内側が下降流、ドラフトチュー
ブ４外側が上昇流となる流れが発生し、上昇流および下
降流はドラフトチューブ４の上端と下端でそれぞれＵタ
ーンするので全体としてドラフトチューブ内側と外側と
の間を循環する循環流が発生することになる。ドラフト
チューブ外側の上昇流は、流速が十分遅く制御されてお
り、外から目に見える程度の大きさく径が０．１ｍ１ｌ
ｌ程度の結晶粒〉以上の結晶は該上昇流によって多少舞
い上っても、ドラフトチューブ上端を越えて上記循環流
と共に循環を起すことはない。これはドラフトチューブ
４の上端と同じ高さに結晶缶の外壁に設けられた図示し
ないガラス窓から循環流の流れ状態を見ることによって
確認できる。上昇流の流速は撹拌翼１８の回転数または
／および翼ピツチ角を調節することにより制御される。When the stirring blades 18 are rotated, a downward flow is generated inside the draft tube 4 and an upward flow is generated outside the draft tube 4, as shown by the arrow 20 in FIG. Since the upper and lower ends each make a U-turn, a circulating flow is generated that circulates between the inside and outside of the draft tube as a whole. The upward flow outside the draft tube is controlled at a sufficiently slow flow rate and is large enough to be visible from the outside, with a diameter of 0.1ml.
Even if the crystals having a size of about 1 or more are slightly blown up by the upward flow, they do not cross the upper end of the draft tube and circulate with the circulation flow. This can be confirmed by observing the flow state of the circulating flow through a glass window (not shown) provided on the outer wall of the crystal can at the same height as the upper end of the draft tube 4. The flow rate of the upward flow is controlled by adjusting the rotation speed and/or blade pitch angle of the stirring blades 18.
結晶缶１がこのように運転されるので、結晶１９は第１
図に示すように撹拌翼の直下部分を除く結晶缶下方に滞
溜し、晶析により結晶が成長する。従って結晶１９が撹
拌翼１８と接触することがないので結晶１９の損傷が起
らずしかも液の循環が十分性われるので結晶の成長も十
分速い。Since the crystal can 1 is operated in this way, the crystal 19 is
As shown in the figure, it accumulates in the lower part of the crystallizer except for the part directly below the stirring blade, and crystals grow by crystallization. Therefore, since the crystal 19 does not come into contact with the stirring blade 18, the crystal 19 is not damaged, and the liquid is sufficiently circulated, so that the crystal grows sufficiently quickly.
以上述べたように本発明の結晶缶の運転方法は以下の効
果があ、る。As described above, the method of operating a crystallizer according to the present invention has the following effects.
（１） 結晶が撹拌翼と接触しないので、結晶が損傷
されることがなく、製品結晶の品質が優れている。(1) Since the crystal does not come into contact with the stirring blade, the crystal is not damaged and the quality of the crystal product is excellent.
■ 循環流の流動は十分性われ、過飽和の溶液の結晶と
の接触は十分性われるので結晶の成長は従来とほぼ同様
の成長速度が得られる。■ The circulation flow is sufficiently controlled and the contact of the supersaturated solution with the crystals is maintained sufficiently, so that the crystal growth rate is almost the same as that of the conventional method.
第１図は結晶化装置における結晶缶の本発明の運転方法
を示す説明図（フローシート）、第２図は結晶缶の従来
の運転方法を示すフローシートである。
１・・・・・・結 晶 缶
４・・・・・・ドラフトチューブ
６・・・・・・セットリング域
１８・・・・・・撹 拌 翼
第１図
第２図FIG. 1 is an explanatory diagram (flow sheet) showing a method of operating a crystal can in a crystallization apparatus according to the present invention, and FIG. 2 is a flow sheet showing a conventional method of operating a crystal can. 1... Crystal can 4... Draft tube 6... Settling area 18... Stirring blade Figure 1 Figure 2
Claims (1)
と、該ドラフトチューブを囲繞して設けられ、循環域と
セットリング域を分離する筒状のバッフルプレートと、
ドラフトチューブ内下方に設けられ、ドラフトチューブ
内側と外側との間を循環する循環流を起す撹拌翼とを備
えた結晶缶を用いて結晶を析出させる結晶缶の運転方法
において、上記撹拌翼により発生する循環流はドラフト
チューブ内側が下降流、ドラフトチューブ外側が上昇流
となつており、且つ撹拌翼の回転数および／またはピッ
チが調節されて、ドラフトチューブ外側の上昇流の流速
は、上昇流により所要大きさ以上の結晶粒が舞い上りド
ラフトチューブ上端を越えて循環する流速より小さくな
つていることを特徴とする結晶缶の運転方法。a draft tube with open upper and lower ends that stands in the center of the can; a cylindrical baffle plate that surrounds the draft tube and separates a circulation area and a settling area;
In a method of operating a crystallizer in which crystals are precipitated using a crystallizer equipped with a stirring blade which is provided in the lower part of the draft tube and generates a circulating flow between the inside and outside of the draft tube, The circulating flow is a downward flow on the inside of the draft tube and an upward flow on the outside of the draft tube, and the rotation speed and/or pitch of the stirring blades is adjusted so that the velocity of the upward flow on the outside of the draft tube is increased by the upward flow. A method of operating a crystal can, characterized in that crystal grains larger than a required size fly up and circulate at a flow rate lower than the flow rate over the upper end of a draft tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62040199A JPS63209702A (en) | 1987-02-25 | 1987-02-25 | Method for operating crystallizer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62040199A JPS63209702A (en) | 1987-02-25 | 1987-02-25 | Method for operating crystallizer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63209702A true JPS63209702A (en) | 1988-08-31 |
Family
ID=12574113
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62040199A Pending JPS63209702A (en) | 1987-02-25 | 1987-02-25 | Method for operating crystallizer |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63209702A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994019083A1 (en) * | 1993-02-17 | 1994-09-01 | China Petro-Chemical Corporation | A process for preparing high purity and large size crystals, by eliminating fine crystals in crystal slurry in crystallizer |
| WO2001091874A1 (en) * | 2000-05-29 | 2001-12-06 | Basf Aktiengesellschaft | Device for producing crystals |
| US6752579B2 (en) | 1995-07-19 | 2004-06-22 | Hitachi, Ltd. | Vacuum processing apparatus and semiconductor manufacturing line using the same |
| JP2011524804A (en) * | 2008-06-18 | 2011-09-08 | ジーイーエー メッソ ゲーエムベーハー | Method and apparatus for continuously producing crystals having a stable particle size distribution |
| CN105664521A (en) * | 2016-02-25 | 2016-06-15 | 多氟多化工股份有限公司 | Dynamic crystallization equipment and dynamic crystallization method |
| CN106422400A (en) * | 2016-10-18 | 2017-02-22 | 阿坝州高远锂电材料有限公司 | Crystallizer |
| CN117919766A (en) * | 2024-03-22 | 2024-04-26 | 山西磊鑫化工股份有限公司 | Reaction crystallization equipment for nitrate production |
| CN117919766B (en) * | 2024-03-22 | 2024-06-04 | 山西磊鑫化工股份有限公司 | Reaction crystallization equipment for nitrate production |
-
1987
- 1987-02-25 JP JP62040199A patent/JPS63209702A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1994019083A1 (en) * | 1993-02-17 | 1994-09-01 | China Petro-Chemical Corporation | A process for preparing high purity and large size crystals, by eliminating fine crystals in crystal slurry in crystallizer |
| US7201551B2 (en) | 1995-07-19 | 2007-04-10 | Hitachi, Ltd. | Vacuum processing apparatus and semiconductor manufacturing line using the same |
| US6895685B2 (en) | 1995-07-19 | 2005-05-24 | Hitachi, Ltd. | Vacuum processing apparatus and semiconductor manufacturing line using the same |
| US7347656B2 (en) | 1995-07-19 | 2008-03-25 | Hitachi, Ltd. | Vacuum processing apparatus and semiconductor manufacturing line using the same |
| US6752580B2 (en) | 1995-07-19 | 2004-06-22 | Hitachi, Ltd. | Vacuum processing apparatus and semiconductor manufacturing line using the same |
| US6752579B2 (en) | 1995-07-19 | 2004-06-22 | Hitachi, Ltd. | Vacuum processing apparatus and semiconductor manufacturing line using the same |
| US6962472B2 (en) | 1995-07-19 | 2005-11-08 | Hitachi, Ltd. | Vacuum processing apparatus and semiconductor manufacturing line using the same |
| US7056356B2 (en) | 2000-05-29 | 2006-06-06 | Basf Aktiengesellschaft | Process for producing crystals |
| CZ303032B6 (en) * | 2000-05-29 | 2012-03-07 | Basf Aktiengesellschaft | Method for crystallizing substances from solutions or dispersions |
| JP2003534129A (en) * | 2000-05-29 | 2003-11-18 | ビーエーエスエフ アクチェンゲゼルシャフト | Equipment for crystal production |
| WO2001091874A1 (en) * | 2000-05-29 | 2001-12-06 | Basf Aktiengesellschaft | Device for producing crystals |
| JP2011524804A (en) * | 2008-06-18 | 2011-09-08 | ジーイーエー メッソ ゲーエムベーハー | Method and apparatus for continuously producing crystals having a stable particle size distribution |
| CN105664521A (en) * | 2016-02-25 | 2016-06-15 | 多氟多化工股份有限公司 | Dynamic crystallization equipment and dynamic crystallization method |
| CN105664521B (en) * | 2016-02-25 | 2018-10-16 | 多氟多化工股份有限公司 | A kind of dynamic crystallization equipment and dynamic crystallization method |
| CN106422400A (en) * | 2016-10-18 | 2017-02-22 | 阿坝州高远锂电材料有限公司 | Crystallizer |
| CN106422400B (en) * | 2016-10-18 | 2018-08-28 | 阿坝州高远锂电材料有限公司 | A kind of crystallizer |
| CN117919766A (en) * | 2024-03-22 | 2024-04-26 | 山西磊鑫化工股份有限公司 | Reaction crystallization equipment for nitrate production |
| CN117919766B (en) * | 2024-03-22 | 2024-06-04 | 山西磊鑫化工股份有限公司 | Reaction crystallization equipment for nitrate production |
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