JP3143866B2 - Crystallization / separation equipment - Google Patents
Crystallization / separation equipmentInfo
- Publication number
- JP3143866B2 JP3143866B2 JP7597497A JP7597497A JP3143866B2 JP 3143866 B2 JP3143866 B2 JP 3143866B2 JP 7597497 A JP7597497 A JP 7597497A JP 7597497 A JP7597497 A JP 7597497A JP 3143866 B2 JP3143866 B2 JP 3143866B2
- Authority
- JP
- Japan
- Prior art keywords
- crystal
- valve body
- nitric acid
- acid solution
- container
- 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.)
- Expired - Lifetime
Links
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
Description
【0001】[0001]
【発明の属する技術分野】本発明は、使用済核燃料を溶
解したUとPuを含む硝酸溶液、或いはピューレックス
溶媒抽出プロセスにおいて共除染・分配工程から得られ
るU或いはPuを含む硝酸溶液を冷却して硝酸化合物結
晶を析出させ、これを分離する晶析・分離装置に関する
ものである。The present invention relates to a method for cooling a nitric acid solution containing U and Pu in which spent nuclear fuel is dissolved, or a nitric acid solution containing U or Pu obtained from a co-decontamination and distribution step in a purex solvent extraction process. The present invention relates to a crystallization / separation device for precipitating a nitric acid compound crystal and separating the same.
【0002】[0002]
【従来の技術】使用済核燃料の再処理法としては溶媒抽
出法を主体としたピューレックス法があり、この溶媒抽
出法は現在のところ、多くの良好な実績が得られ、最良
のプロセスと判断される。しかし、この再処理法は工程
全体を溶媒抽出法のみで行うこととしているため、工程
が複雑となり装置及び設備の数が多くなるという改良す
べき点があった。またこの再処理方法は有機溶媒を使用
するため、溶媒洗浄廃液や廃溶媒等の溶媒に係わる廃棄
物が発生し、またそれを分解処理又は無機化処理するた
めの設備が必要となる等の溶媒抽出法特有の特徴があ
り、将来の再処理プロセスを考慮した場合、更なる工程
・設備の簡素化、廃棄物の低減化を行う等の再処理プロ
セスの改良が望まれている。2. Description of the Related Art As a method of reprocessing spent nuclear fuel, there is a purex method mainly based on a solvent extraction method. At present, many good results have been obtained, and the solvent extraction method has been judged to be the best process. Is done. However, in this reprocessing method, since the entire process is performed only by the solvent extraction method, there is a point to be improved that the process becomes complicated and the number of apparatuses and equipment increases. In addition, since this reprocessing method uses an organic solvent, a solvent-related waste such as a solvent washing waste liquid and a waste solvent is generated, and a solvent for decomposing or mineralizing the solvent is required. There is a feature unique to the extraction method, and when a future reprocessing process is considered, improvement of the reprocessing process such as further simplification of processes and equipment and reduction of waste is desired.
【0003】この改良を図るため、本出願人は従来のピ
ューレックス法において、水平又は傾斜して設けられた
外管の内部に駆動部で回転駆動される内管が設けられ、
外管の上部にUとPuを含む硝酸溶液等を供給する原料
供給口と硝酸溶液冷却用の冷媒を供給する複数の冷媒供
給口が設けられ、更に内管の外周面に案内羽根が設けら
れた「晶析装置」を特許出願した(特開平7−1402
94号)。この晶析装置では、外管の他端が外管キャッ
プにより塞がれ、この外管キャップの上部及び下部に母
液抜出し部及び結晶取出し部がそれぞれ形成される。冷
媒供給口が外管の管上部に長手方向に所定の間隔をあけ
て複数設けられ、この供給口から液体窒素やドライアイ
ス等の冷媒が供給されて外管内の硝酸溶液が冷却される
ようになっている。[0003] In order to achieve this improvement, the present applicant has, in the conventional Purex method, an inner pipe that is rotationally driven by a drive unit inside a horizontal or inclined outer pipe,
A raw material supply port for supplying a nitric acid solution containing U and Pu and a plurality of refrigerant supply ports for supplying a cooling medium for cooling the nitric acid solution are provided at an upper portion of the outer tube, and a guide blade is provided on an outer peripheral surface of the inner tube. Filed a patent application for "Crystallizer" (Japanese Unexamined Patent Publication No.
No. 94). In this crystallization apparatus, the other end of the outer tube is closed by an outer tube cap, and a mother liquor extracting portion and a crystal extracting portion are formed on the upper and lower portions of the outer tube cap, respectively. A plurality of coolant supply ports are provided at predetermined intervals in the longitudinal direction at the top of the outer tube, and a coolant such as liquid nitrogen or dry ice is supplied from this supply port to cool the nitric acid solution in the outer tube. Has become.
【0004】このように構成された晶析装置では、外管
と内管で挟まれる限られた空間で硝酸溶液が冷却されて
硝酸化合物結晶が析出し、結晶を含むスラリーが生成さ
れる。このスラリーに含まれる結晶は連続して結晶取出
し部から取出され、同時にスラリーの母液は母液抜出し
部より取出される。この結果、臨界管理上の制限があっ
てもこれに適合し、連続的にかつ高い除染効率で硝酸化
合物結晶を得ることができるようになっている。In the crystallizer configured as described above, the nitric acid solution is cooled in a limited space between the outer tube and the inner tube to precipitate nitric acid compound crystals, thereby producing a slurry containing the crystals. The crystals contained in the slurry are continuously taken out from the crystal take-out section, and at the same time, the mother liquor of the slurry is taken out from the mother liquor take-out section. As a result, even if there is a limitation on the criticality management, the nitrate compound crystal can be obtained continuously and with high decontamination efficiency.
【0005】[0005]
【発明が解決しようとする課題】しかし、上記従来の晶
析装置では、硝酸溶液を冷却することにより析出した硝
酸化合物結晶が沈降するのに比較的多くの時間を要する
問題点があった。また、上記従来の晶析装置では、結晶
取出し部が外管キャップの下部に設けられているため、
この結晶取出し部から硝酸化合物結晶を取出すときに結
晶とともに硝酸溶液の母液も排出される。この結果、結
晶の粒径より小さいメッシュのスクリーン等を用いて結
晶と母液とを分離する必要があり、装置が大型化する問
題点があった。本発明の目的は、短時間でかつ同時に硝
酸溶液の冷却晶析と固液分離を行うことができ、この冷
却晶析及び固液分離のプロセスを大幅にコンパクト化で
きる晶析・分離装置を提供することにある。However, in the above-mentioned conventional crystallizer, there is a problem that it takes a relatively long time for the nitrate compound crystals precipitated by cooling the nitric acid solution to settle. Further, in the above-mentioned conventional crystallizer, since the crystal take-out part is provided below the outer tube cap,
When taking out the nitrate compound crystal from the crystal take-out part, the mother liquor of the nitric acid solution is discharged together with the crystal. As a result, it is necessary to separate the crystal and the mother liquor using a mesh screen or the like smaller than the crystal grain size, and there has been a problem that the apparatus becomes large. An object of the present invention is to provide a crystallization / separation apparatus which can perform cooling crystallization and solid-liquid separation of a nitric acid solution in a short time and simultaneously, and can greatly reduce the process of cooling crystallization and solid-liquid separation. Is to do.
【0006】[0006]
【課題を解決するための手段】請求項1に係る発明は、
図1に示すように、使用済核燃料を溶解したUとPuを
含む硝酸溶液17、或いはピューレックス溶媒抽出プロ
セスにおいて共除染・分配工程から得られるU或いはP
uを含む硝酸溶液17を冷却して硝酸化合物結晶17b
を析出させ硝酸化合物結晶17bを含むスラリーから硝
酸化合物結晶17bを分離する晶析・分離装置の改良で
ある。その特徴ある構成は、下端に末広開口部11eが
形成されたアッパコーン11aと上端に末広開口部11
fが形成されたロアコーン11bとを有し各末広開口部
11e,11fの周縁を互いに接合することにより内部
に硝酸溶液17を貯留可能に形成されかつアッパコーン
11aの上端及びロアコーン11bの下端に鉛直方向に
延びて接続されたシャフト12を中心に回転可能な回転
容器11と、アッパコーン11aの周壁内部からロアコ
ーン11bの周壁内部にかけて形成され回転容器11内
の硝酸溶液17を冷却して硝酸化合物結晶17bを析出
する冷却液が通過可能な冷却液通路11cと、回転容器
11の最外周部に形成され回転容器11の回転による遠
心力にて最外周部内面に堆積した硝酸化合物結晶17b
を排出可能な結晶出口11dと、結晶出口11dを開放
可能に閉止する弁開閉機構16とを備えたところにあ
る。The invention according to claim 1 is
As shown in FIG. 1, a nitric acid solution 17 containing U and Pu in which spent nuclear fuel is dissolved, or U or P obtained from a co-decontamination and distribution step in a purex solvent extraction process.
cooling the nitric acid solution 17 containing u
This is an improvement of a crystallization / separation apparatus for separating nitrate compound crystals 17b from a slurry containing nitrate compound crystals 17b by precipitating the same. Its characteristic configuration is that an upper cone 11a having a divergent opening 11e at the lower end and a divergent opening 11 at the upper end.
and a lower cone 11b in which the f is formed. The peripheral edges of the divergent openings 11e and 11f are joined to each other so that the nitric acid solution 17 can be stored therein, and the upper end of the upper cone 11a and the lower end of the lower cone 11b are vertically arranged. A rotating container 11 rotatable about a shaft 12 connected to and connected to the inner wall of the upper cone 11a and a lower wall of the lower cone 11b. The nitric acid solution 17 in the rotating container 11 is cooled to form a nitrate compound crystal 17b. A cooling liquid passage 11c through which the precipitated cooling liquid can pass, and a nitric acid compound crystal 17b formed on the outermost peripheral portion of the rotary container 11 and deposited on the inner surface of the outermost peripheral portion by centrifugal force generated by rotation of the rotary container 11
And a valve opening / closing mechanism 16 for opening and closing the crystal outlet 11d.
【0007】この請求項1に係る晶析・分離装置では、
回転容器11をシャフト12を中心に回転させた状態
で、冷却液通路11cに冷却液を供給しながら回転容器
11に硝酸溶液17を供給すると、回転容器11内の硝
酸溶液17は冷却液により冷却されて硝酸化合物結晶1
7bが析出し、この硝酸化合物結晶17bは回転容器1
1の回転による遠心力にて回転容器11の最外周部内面
に堆積する。次に回転容器11の回転を停止して回転容
器11内の硝酸溶液17の母液17aを排出した後、再
び回転容器11を回転させて弁開閉機構16により結晶
出口11dを開放すると、上記結晶17bは遠心力によ
り結晶出口11dから回転容器11外に排出される。In the crystallization / separation apparatus according to the first aspect,
When the nitric acid solution 17 is supplied to the rotating container 11 while supplying the cooling liquid to the cooling liquid passage 11 c while the rotating container 11 is rotated about the shaft 12, the nitric acid solution 17 in the rotating container 11 is cooled by the cooling liquid. Nitrate compound crystal 1
7b is precipitated, and the nitric acid compound crystal 17b is
Due to the centrifugal force caused by the rotation of No. 1, it is deposited on the inner surface of the outermost peripheral portion of the rotating container 11. Next, after the rotation of the rotating container 11 is stopped and the mother liquor 17a of the nitric acid solution 17 in the rotating container 11 is discharged, the rotating container 11 is rotated again to open the crystal outlet 11d by the valve opening / closing mechanism 16, and the crystal 17b Is discharged out of the rotating container 11 from the crystal outlet 11d by centrifugal force.
【0008】請求項2に係る発明は、請求項1に係る発
明であって、更に図1に示すように、弁開閉機構16
が、回転容器11に支持ピン29dを介して略中央が枢
着された弁本体29と、弁本体29の先端に形成され回
転容器11の結晶出口11dに密着可能な弁座部29a
と、弁本体29の基端に連結され支持ピン29dを中心
に弁本体29を揺動することにより弁座部29aを結晶
出口11dに密着又は結晶出口11dから離脱させる弁
本体駆動手段30と、弁本体29のうちこの弁本体29
の基端と支持ピン29dとの間に設けられ弁本体29が
回転容器11とともに回転するときに発生する遠心力に
より弁座部29aが結晶出口11dに密着する方向に弁
本体29を付勢するウエイト29bとを備えたことを特
徴とする。この請求項2に係る晶析・分離装置では、弁
開閉機構16により結晶出口11dが閉止され、かつ弁
本体29が回転容器11とともに回転するときに、ウエ
イト29bに発生する遠心力が弁本体29を支持ピン2
9dを中心に所定の方向に回転させるように付勢する。
上記所定の方向は弁座部29aが結晶出口11dに密着
する方向であり、これにより弁座部29aの結晶出口1
1dへの密着性が向上する。The invention according to claim 2 is the invention according to claim 1, and further includes a valve opening / closing mechanism 16 as shown in FIG.
A valve body 29 pivotally connected at a substantially center to the rotary container 11 via a support pin 29d; and a valve seat portion 29a formed at the tip of the valve body 29 and capable of closely contacting the crystal outlet 11d of the rotary container 11.
A valve main body driving means 30 connected to the base end of the valve main body 29 and swinging the valve main body 29 around the support pin 29d to bring the valve seat portion 29a into close contact with the crystal outlet 11d or to separate from the crystal outlet 11d; The valve body 29 of the valve body 29
The valve seat 29a is urged in a direction in which the valve seat portion 29a comes into close contact with the crystal outlet 11d by centrifugal force generated when the valve body 29 rotates together with the rotary container 11 and is provided between the base end of the valve body and the support pin 29d. And a weight 29b. In the crystallization / separation apparatus according to the second aspect, when the crystallization outlet 11d is closed by the valve opening / closing mechanism 16 and the valve body 29 rotates together with the rotary container 11, the centrifugal force generated in the weight 29b causes the valve body 29 to rotate. The support pin 2
It is urged to rotate around 9d in a predetermined direction.
The predetermined direction is a direction in which the valve seat 29a is in close contact with the crystal outlet 11d.
Adhesion to 1d is improved.
【0009】[0009]
【発明の実施の形態】次に本発明の実施の形態を図面に
基づいて詳しく説明する。図1及び図2に示すように、
晶析・分離装置10は、アッパコーン11aとロアコー
ン11bとを互いに接合して形成されシャフト12を中
心に回転可能な回転容器11と、アッパコーン11aの
周壁内部からロアコーン11bの周壁内部にかけて形成
された冷却液通路11cと、回転容器11の最外周部に
形成された結晶出口11dと、結晶出口11dを開放可
能に閉止する弁開閉機構16とを備える。アッパコーン
11aは下端に末広開口部11eを有し、ロアコーン1
1bは上端に末広開口部11fを有し、回転容器11は
上記各末広開口部11e,11fを互いに溶接にて接合
することにより内部に硝酸溶液17を貯留可能に構成さ
れる。硝酸溶液17は使用済核燃料を再処理したUとP
uを含む硝酸溶液、或いはピューレックス溶媒抽出プロ
セスにおいて共除染・分配工程から得られるU或いはP
uを含む硝酸溶液である。シャフト12は下端がアッパ
コーン11aの上端に溶接により接続されたアッパシャ
フト13と、上端がロアコーン11bの下端に溶接によ
り接続されたロアシャフト14とを有し、アッパシャフ
ト13及びロアシャフト14はこれらの軸線が同一鉛直
線上に位置するようにアッパコーン11a及びロアコー
ン11bにそれぞれ接続される。Embodiments of the present invention will now be described in detail with reference to the drawings. As shown in FIGS. 1 and 2,
The crystallization / separation device 10 includes a rotating container 11 formed by joining an upper cone 11a and a lower cone 11b to each other and rotatable about a shaft 12, and a cooling formed from the inner peripheral wall of the upper cone 11a to the inner peripheral wall of the lower cone 11b. It has a liquid passage 11c, a crystal outlet 11d formed at the outermost periphery of the rotary container 11, and a valve opening / closing mechanism 16 for opening and closing the crystal outlet 11d. The upper cone 11a has a divergent opening 11e at the lower end.
1b has a divergent opening 11f at the upper end, and the rotary container 11 is configured to be able to store the nitric acid solution 17 therein by welding the divergent openings 11e and 11f to each other by welding. The nitric acid solution 17 contains U and P obtained by reprocessing spent nuclear fuel.
nitric acid solution containing u, or U or P obtained from the co-decontamination and distribution step in the Purex solvent extraction process
This is a nitric acid solution containing u. The shaft 12 has an upper shaft 13 whose lower end is connected to the upper end of the upper cone 11a by welding, and a lower shaft 14 whose upper end is connected to the lower end of the lower cone 11b by welding. The upper shaft 13 and the lower shaft 14 They are connected to the upper cone 11a and the lower cone 11b, respectively, so that the axes are located on the same vertical line.
【0010】また回転容器11は下端がベース18に取
付けられたケース19に収容される。ロアシャフト14
はベース18に軸受21を介して回転可能に取付けら
れ、アッパシャフト13はケース19の上端に軸受22
を介して回転可能に取付けられる。またロアシャフト1
4にはこのシャフト14の軸線に一致して硝酸溶液17
を回転容器11内に供給するための原液供給通路14a
が形成され、アッパシャフト13にはこのシャフト13
の軸線に一致して硝酸溶液17の母液17aを回転容器
11から排出する母液排出通路13aが形成される。原
液供給通路14aの上端はロアシャフト14の上面に達
して回転容器11内に臨み、下端はロアシャフト14の
下面に達する。母液排出通路13aの下端はアッパシャ
フト13の下面に達して回転容器11内に臨み、上端は
アッパシャフト13の下端から所定の距離だけ上方のア
ッパシャフト13側面に達する。なお、ロアシャフトの
上面には原液供給通路の上端を覆うスクリーンを設ける
ことが好ましい。このスクリーンは硝酸溶液を通過可能
かつ硝酸化合物結晶を通過不能な所定のメッシュを有す
る。The rotating container 11 is accommodated in a case 19 whose lower end is attached to a base 18. Lower shaft 14
Is rotatably mounted on a base 18 via a bearing 21, and the upper shaft 13
It is rotatably mounted via. In addition, lower shaft 1
4 has a nitric acid solution 17 corresponding to the axis of the shaft 14.
Solution supply passage 14a for supplying
Is formed on the upper shaft 13.
And a mother liquor discharge passage 13a for discharging the mother liquor 17a of the nitric acid solution 17 from the rotary container 11 is formed. The upper end of the stock solution supply passage 14a reaches the upper surface of the lower shaft 14 and faces the inside of the rotary container 11, and the lower end reaches the lower surface of the lower shaft 14. The lower end of the mother liquor discharge passage 13a reaches the lower surface of the upper shaft 13 and faces the inside of the rotating container 11, and the upper end reaches the side surface of the upper shaft 13 a predetermined distance above the lower end of the upper shaft 13. Preferably, a screen is provided on the upper surface of the lower shaft to cover the upper end of the stock solution supply passage. The screen has a predetermined mesh that can pass through the nitric acid solution and cannot pass through the nitrate compound crystal.
【0011】アッパシャフト13はケース19の上端か
ら上方に突出し、このシャフト13の突出下部には従動
プーリ23が嵌着される。またケース19の上部外面に
はブラケット24を介してモータ26が取付けられ、こ
のモータ26の出力軸26aには駆動プーリ27が嵌着
される。駆動プーリ27と従動プーリ23にはベルト2
8が掛け渡される。冷却液通路11cには回転容器11
内の硝酸溶液17を冷却して硝酸化合物結晶17bを析
出する冷却液(図示せず)が通過可能に構成される。冷
却液としてはエチレングリコールと水の混合物等が用い
られる。冷却液通路11cの上端はアッパシャフト13
に鉛直方向に延びて形成され冷却液通路11cに冷却液
を供給する冷却液供給通路13bに連通し、冷却液通路
11cの下端はロアシャフト14に鉛直方向に延びて形
成され冷却液通路11cから冷却液を排出する冷却液排
出通路14bに連通する。冷却液供給通路13bはアッ
パシャフト13の軸線からずれた位置にこの軸線と平行
に形成され、その上端はアッパシャフト13の上面に達
する。冷却液排出通路14bはロアシャフト14の軸線
からずれた位置にこの軸線と平行に形成され、その下端
はロアシャフト14の下面に達する。The upper shaft 13 protrudes upward from the upper end of the case 19, and a driven pulley 23 is fitted to a protruding lower portion of the shaft 13. A motor 26 is mounted on the upper outer surface of the case 19 via a bracket 24, and a drive pulley 27 is fitted on an output shaft 26 a of the motor 26. The driving pulley 27 and the driven pulley 23 have a belt 2
8 is passed over. The rotating vessel 11 is provided in the coolant passage 11c.
A cooling liquid (not shown) for cooling the nitric acid solution 17 therein to precipitate the nitric acid compound crystals 17b is configured to pass therethrough. As the cooling liquid, a mixture of ethylene glycol and water is used. The upper end of the coolant passage 11c is
The coolant passage 11c is formed to extend vertically and communicates with the coolant supply passage 13b that supplies coolant to the coolant passage 11c. The lower end of the coolant passage 11c extends vertically to the lower shaft 14 and extends from the coolant passage 11c. It communicates with a coolant discharge passage 14b for discharging the coolant. The coolant supply passage 13 b is formed at a position deviated from the axis of the upper shaft 13 and in parallel with the axis, and the upper end reaches the upper surface of the upper shaft 13. The coolant discharge passage 14 b is formed at a position deviated from the axis of the lower shaft 14 in parallel with the axis, and the lower end thereof reaches the lower surface of the lower shaft 14.
【0012】弁開閉機構16は、回転容器11に枢着さ
れた弁本体29と、弁本体29の先端に形成され回転容
器11の結晶出口11dに密着可能な弁座部29aと、
弁本体29の基端に連結された弁本体駆動手段30と、
弁本体29に設けられたウエイト29bとを備える。弁
本体29は略クランク状に形成され、その中央下部がア
ッパコーン11aの外周面にブラケット29c及び支持
ピン29dを介して揺動可能に取付けられる。弁座部2
9aは結晶出口11dに密着可能に構成され、結晶出口
11dへの密着時に回転容器11内の硝酸溶液17の漏
出を阻止するように構成される。弁本体駆動手段30は
アッパシャフト13の下部に固定されたピストン30a
と、このピストン30aを収容しかつアッパシャフト1
3及びピストン30aに対して鉛直方向に摺動するシリ
ンダ30bと、ピストン30aの上面とシリンダ30b
の内部上面との間に介装されシリンダ30bを押上げる
ように付勢するシリンダ用ばね30cとを有する。The valve opening / closing mechanism 16 includes a valve main body 29 pivotally attached to the rotary container 11, a valve seat portion 29a formed at the tip of the valve main body 29 and capable of closely contacting a crystal outlet 11d of the rotary container 11,
Valve body driving means 30 connected to the base end of the valve body 29;
A weight 29b provided on the valve body 29. The valve body 29 is formed in a substantially crank shape, and a lower center portion thereof is swingably attached to an outer peripheral surface of the upper cone 11a via a bracket 29c and a support pin 29d. Valve seat 2
9a is configured so as to be able to adhere to the crystal outlet 11d, and is configured to prevent leakage of the nitric acid solution 17 in the rotating container 11 when the crystal outlet 9d is in close contact with the crystal outlet 11d. The valve body driving means 30 includes a piston 30a fixed to a lower portion of the upper shaft 13.
And the upper shaft 1 that accommodates the piston 30a and
3 and a cylinder 30b that slides vertically with respect to the piston 30a, and an upper surface of the piston 30a and the cylinder 30b.
And a cylinder spring 30c urged to push up the cylinder 30b.
【0013】シリンダ30bの下面には水平方向に延び
る長孔30eが形成された係合部材30dが突設され、
この長孔30eに弁本体29の基端に固着された係合ピ
ン29eが摺動可能に挿入される。またアッパシャフト
13にはこのシャフト13の軸心に一致して油通路13
cが形成され、この油通路13cの下端はシリンダ30
b内部のうちピストン30aの下方に連通し、上端はア
ッパシャフト13の上面に達する。ウエイト29bは弁
本体29のうちこの弁本体29の基端と支持ピン29d
との間に弁本体29と一体的に設けられ、弁本体29が
回転容器11とともに回転するときに発生する遠心力に
より弁座部29aが結晶出口11dに密着する方向に弁
本体29を付勢するように構成される。弁本体29は回
転容器11の回転バランスを考慮してシャフト12を中
心に対称に複数設けられることが好ましく、結晶出口1
1dや係合部材30d等は弁本体29と同数形成され
る。An engaging member 30d is formed on the lower surface of the cylinder 30b and has an elongated hole 30e extending in the horizontal direction.
An engagement pin 29e fixed to the base end of the valve body 29 is slidably inserted into the elongated hole 30e. In addition, the upper shaft 13 has an oil passage 13 which coincides with the axis of the shaft 13.
c is formed, and the lower end of the oil passage 13c is
The inside of b communicates below the piston 30a, and the upper end reaches the upper surface of the upper shaft 13. The weight 29b is provided between the base end of the valve body 29 and the support pin 29d.
And the valve body 29 is urged in a direction in which the valve seat portion 29a comes into close contact with the crystal outlet 11d by centrifugal force generated when the valve body 29 rotates together with the rotary container 11. It is configured to It is preferable that a plurality of valve bodies 29 are provided symmetrically around the shaft 12 in consideration of the rotational balance of the rotary container 11.
1d, the engagement member 30d, and the like are formed in the same number as the valve body 29.
【0014】図3に示すように、アッパシャフト13の
上端には油通路13cを上方に延ばすための小径パイプ
13dが突設される。またアッパシャフト13の上端に
はロアフランジ13eが嵌着され、このフランジ13e
には冷却液供給通路13bに連通する第1連通孔13f
が形成される。ロアフランジ13eの上端及び小径パイ
プ13dの上端には、冷却液供給通路13bに連通する
冷却液供給口31aと油通路13cに連通する油給排口
31bとが形成された公知の第1回転継手31が接続さ
れる。第1回転継手31の冷却液供給口31aには冷却
液供給パイプ38を介して冷却液ポンプ(図示せず)が
接続され、油給排口31bには油供給パイプ39を介し
て油ポンプ(図示せず)が接続される。即ち第1回転継
手31は、回転するアッパシャフト13に形成された冷
却液供給通路13b及び油通路13cに冷却液及び高圧
油を漏出することなくスムーズに供給及び給排できるよ
うになっている。As shown in FIG. 3, a small-diameter pipe 13d for projecting the oil passage 13c upward is provided at the upper end of the upper shaft 13. A lower flange 13e is fitted on the upper end of the upper shaft 13, and this flange 13e
Has a first communication hole 13f communicating with the coolant supply passage 13b.
Is formed. A known first rotary joint 31 in which a cooling liquid supply port 31a communicating with the cooling liquid supply passage 13b and an oil supply / discharge port 31b communicating with the oil passage 13c are formed at the upper end of the lower flange 13e and the upper end of the small diameter pipe 13d. Is connected. A coolant pump (not shown) is connected to the coolant supply port 31a of the first rotary joint 31 via a coolant supply pipe 38, and an oil pump (not shown) is connected to the oil supply / discharge port 31b via an oil supply pipe 39. (Not shown). That is, the first rotary joint 31 can smoothly supply and discharge the coolant and the high-pressure oil without leaking into the coolant supply passage 13b and the oil passage 13c formed in the rotating upper shaft 13.
【0015】第1回転継手31はロアフランジ13eの
上端に取付けられたアッパフランジ32と、アッパフラ
ンジ32に軸受33,33を介して嵌入された円筒部材
34と、円筒部材34の上端に挿着され上記冷却液供給
口31a及び油給排口31bが形成された円柱部材35
とを有する。アッパフランジ32には第1連通孔13f
に連通する第2連通孔32aが形成され、小径パイプ1
3dの上端にはガスケットパッキン36を介して連結パ
イプ37が接続される。また円柱部材35には冷却液供
給口31aに連通する大径の穴35aと、油給排口31
bに連通する小径の穴35bが形成される。大径の穴3
5a及び小径の穴35bには鉛直方向に摺動可能に第1
及び第2シール保持具41,42がそれぞれ挿入され
る。The first rotary joint 31 is attached to an upper flange 32 attached to the upper end of the lower flange 13e, a cylindrical member 34 fitted into the upper flange 32 via bearings 33, 33, and inserted into the upper end of the cylindrical member 34. A cylindrical member 35 having the cooling liquid supply port 31a and the oil supply / discharge port 31b formed therein.
And The first communication hole 13f is formed in the upper flange 32.
A second communication hole 32a communicating with the small diameter pipe 1 is formed.
A connection pipe 37 is connected to the upper end of 3d via a gasket packing 36. The cylindrical member 35 has a large-diameter hole 35 a communicating with the coolant supply port 31 a and an oil supply / discharge port 31.
A small hole 35b communicating with b is formed. Large diameter hole 3
5a and the small-diameter hole 35b are slidable vertically in the first direction.
And the second seal holders 41 and 42 are inserted respectively.
【0016】第1シール保持具41にはアッパフランジ
32の第2連通孔32aと大径の穴35aとを連通する
第3連通孔41aが形成され、この保持具41の下端に
はカーボングラファイトにより形成された円筒状の第1
シール部材51が挿着される。円柱部材35と第1シー
ル保持具41との間には第1ばね61が介装され、この
ばね61の弾性力により第1シール部材51の下面がア
ッパフランジ32の上面に摺動可能に圧接される。第2
シール保持具42には連結パイプ37の孔37aと小径
の穴35bとを連通する第4連通孔42aが形成され、
この保持具42の下端にはカーボングラファイトにより
形成された円筒状の第2シール部材52が挿着される。
円柱部材35と第2シール保持具42との間には第2ば
ね62が介装され、このばね62の弾性力により第2シ
ール部材52の下面が連結パイプ37の上面に摺動可能
に圧接される。図3中の符号71は3ポート2位置切換
えの第1電磁バルブであり、符号72はシリンダ30b
内の高圧油を油タンク(図示せず)に戻す油戻りパイプ
である。第1電磁バルブ71をオンすると高圧油40が
油供給パイプ39及び油通路13cを介してシリンダ3
0b内に供給され、オフするとシリンダ30b内の高圧
油が油通路13c及び油戻りパイプ72を介して排出さ
れるようになっている。The first seal holder 41 is formed with a third communication hole 41a for communicating the second communication hole 32a of the upper flange 32 with the large-diameter hole 35a. The lower end of the holder 41 is made of carbon graphite. Formed cylindrical first
The seal member 51 is inserted. A first spring 61 is interposed between the cylindrical member 35 and the first seal holder 41, and the lower surface of the first seal member 51 is slidably pressed against the upper surface of the upper flange 32 by the elastic force of the spring 61. Is done. Second
A fourth communication hole 42a that connects the hole 37a of the connection pipe 37 and the small-diameter hole 35b is formed in the seal holder 42,
A cylindrical second seal member 52 made of carbon graphite is inserted into the lower end of the holder 42.
A second spring 62 is interposed between the cylindrical member 35 and the second seal holder 42, and the lower surface of the second seal member 52 is slidably pressed against the upper surface of the connecting pipe 37 by the elastic force of the spring 62. Is done. Reference numeral 71 in FIG. 3 is a first solenoid valve that switches between three ports and two positions, and reference numeral 72 is a cylinder 30b.
An oil return pipe that returns high-pressure oil inside the tank to an oil tank (not shown). When the first electromagnetic valve 71 is turned on, the high-pressure oil 40 is supplied to the cylinder 3 via the oil supply pipe 39 and the oil passage 13c.
0b, and when turned off, the high-pressure oil in the cylinder 30b is discharged through the oil passage 13c and the oil return pipe 72.
【0017】また図4に示すように、ロアシャフト14
の下端には冷却液排出通路14bに連通する大径の凹部
14cが形成され、この凹部14cの中央には原液供給
通路14aを下方に延ばすための短管14dが突設され
る。ロアシャフト14の下端及び短管14dの下端に
は、冷却液排出通路14bに連通する冷却液排出口82
aと原液供給通路14aに連通する原液供給口82bと
が形成された第2回転継手82が接続される。この第2
回転継手82は上記第1回転継手31と略同一に構成さ
れる。図4において図3と同一符号は同一部品を示す。
第2回転継手82の冷却液排出口82aには冷却液排出
パイプ83が接続され、原液供給口82bには原液供給
パイプ84が接続される。即ち第2回転継手82は、回
転するロアシャフト14に形成された冷却液排出通路1
4bから冷却液を漏出することなくスムーズに排出で
き、かつ回転するロアシャフト14に形成された原液供
給通路14aに硝酸溶液を漏出することなくスムーズに
供給できるようになっている。図4中の符号92は3ポ
ート2位置切換えの第2電磁バルブであり、符号93は
回転容器内の硝酸溶液の母液を母液タンク(図示せず)
に排出する母液戻りパイプである。第2電磁バルブ92
をオンすると硝酸溶液が原液供給パイプ84及び原液供
給通路14aを介して回転容器内に供給され、オフする
と回転容器内の硝酸溶液の母液が原液供給通路14a及
び母液戻りパイプ93を介して排出されるようになって
いる。Further, as shown in FIG.
A large-diameter concave portion 14c communicating with the cooling liquid discharge passage 14b is formed at the lower end of the lower end, and a short pipe 14d for projecting the stock solution supply passage 14a downward is formed at the center of the concave portion 14c. At the lower end of the lower shaft 14 and the lower end of the short pipe 14d, a coolant discharge port 82 communicating with the coolant discharge passage 14b is provided.
a and a second rotary joint 82 formed with a stock solution supply port 82b communicating with the stock solution supply passage 14a. This second
The rotary joint 82 is configured substantially the same as the first rotary joint 31. 4, the same reference numerals as those in FIG. 3 indicate the same parts.
A coolant discharge pipe 83 is connected to the coolant discharge port 82a of the second rotary joint 82, and a stock solution supply pipe 84 is connected to the stock solution supply port 82b. That is, the second rotary joint 82 is connected to the coolant discharge passage 1 formed in the rotating lower shaft 14.
The cooling liquid can be smoothly discharged from the lower shaft 4b without leaking, and the nitric acid solution can be smoothly supplied to the raw liquid supply passage 14a formed in the rotating lower shaft 14 without leaking. Reference numeral 92 in FIG. 4 denotes a second electromagnetic valve that switches between three ports and two positions, and reference numeral 93 denotes a mother liquor tank (not shown) for storing a mother liquor of the nitric acid solution in the rotary container.
This is the mother liquor return pipe discharged to Second electromagnetic valve 92
Is turned on, the nitric acid solution is supplied into the rotary container via the raw liquid supply pipe 84 and the raw liquid supply passage 14a, and when turned off, the mother liquor of the nitric acid solution in the rotary container is discharged via the raw liquid supply passage 14a and the mother liquid return pipe 93. It has become so.
【0018】図1及び図2に戻って、ベース18上には
シャフト12と同心に、ケース19より僅かに小径の円
筒状の第1仕切壁18aと、回転容器11の外径より僅
かに小径の円筒状の第2仕切壁18bとがそれぞれ立設
される。ケース19と第1仕切壁18aとの間には母液
排出室18cが形成され、第1仕切壁18aと第2仕切
壁18bとの間に結晶排出室18dが形成される。ベー
ス18には母液排出室18cに臨んで母液排出口18e
が形成され、この排出口18eは母液タンクに接続され
る。またベース18には結晶排出室18dに臨んで大径
の結晶排出口18fが形成される。またアッパシャフト
13の母液排出通路13aの上端には母液排出パイプ1
8gの基端が水平方向に延びて接続され、このパイプ1
8gの先端は母液排出室18cに臨む。また硝酸化合物
結晶17bを結晶排出室18dから効率よく排出するた
めに、結晶排出口18fの数を多くしたり、結晶排出口
18fを円弧状の長孔に形成したり、或いはベース19
の上面のうち結晶排出室18dの底面を形成する面を結
晶排出口18fに向って硝酸化合物結晶17bが流下す
るように傾斜面に形成したりすることが好ましい。Returning to FIGS. 1 and 2, a cylindrical first partition wall 18 a having a diameter slightly smaller than the case 19 and a diameter slightly smaller than the outer diameter of the rotary container 11 are provided on the base 18 concentrically with the shaft 12. And the cylindrical second partition wall 18b is erected. A mother liquor discharge chamber 18c is formed between the case 19 and the first partition wall 18a, and a crystal discharge chamber 18d is formed between the first partition wall 18a and the second partition wall 18b. The base 18 has a mother liquor discharge port 18e facing the mother liquor discharge chamber 18c.
Is formed, and this outlet 18e is connected to the mother liquor tank. The base 18 has a large-diameter crystal discharge port 18f facing the crystal discharge chamber 18d. A mother liquor discharge pipe 1 is provided at the upper end of the mother liquor discharge passage 13a of the upper shaft 13.
The base end of 8 g extends in the horizontal direction and is connected.
The tip of 8 g faces the mother liquor discharge chamber 18c. In order to efficiently discharge the nitrate compound crystal 17b from the crystal discharge chamber 18d, the number of the crystal discharge ports 18f is increased, the crystal discharge ports 18f are formed in arc-shaped long holes, or the base 19 is formed.
It is preferable that the surface forming the bottom surface of the crystal discharge chamber 18d is formed as an inclined surface such that the nitrate compound crystal 17b flows down toward the crystal discharge port 18f.
【0019】このように構成された晶析・分離装置の動
作を説明する。先ずモータ26によりシャフト12及び
回転容器11を回転させ、冷却液(図示せず)を第1回
転継手31の冷却液供給口31aから冷却液供給通路1
3bを介して回転容器11の冷却液通路11cに供給す
る。次に第2電磁バルブ92をオンして硝酸溶液17を
第2回転継手82の原液供給口82bから原液供給通路
14aを介して回転容器11内に一定の供給速度で供給
する。このとき第1電磁バルブ71はオフしているの
で、シリンダ30b内に高圧油40(図2)が供給され
ず、シリンダ30bはシリンダ用ばね30cの弾性力に
より最も上昇した状態に保たれ、弁本体29の弁座部2
9aが結晶出口14dに密着して結晶出口14dを閉止
する。また弁本体29は回転容器11とともに回転する
ため、ウエイト29bに発生する遠心力が弁本体29を
支持ピン29dを中心に図1の破線矢印の方向に回転さ
せるように付勢する。この結果、弁座部29aの結晶出
口11dへの密着性が向上する。回転容器11内に順次
供給される硝酸溶液17は冷却液により冷却されて硝酸
化合物結晶17bが析出し、この硝酸化合物結晶17b
は回転容器11の回転による遠心力にて回転容器11の
最外周部内面に堆積する。また回転容器11内の硝酸溶
液17の母液17aは母液排出通路13a、母液排出パ
イプ18g及び母液排出室18cを介して母液排出口1
8eから排出される。The operation of the crystallization / separation apparatus thus configured will be described. First, the shaft 12 and the rotary container 11 are rotated by the motor 26, and a coolant (not shown) is supplied from the coolant supply port 31 a of the first rotary joint 31 to the coolant supply passage 1.
The liquid is supplied to the cooling liquid passage 11c of the rotary container 11 through 3b. Next, the second electromagnetic valve 92 is turned on to supply the nitric acid solution 17 from the stock solution supply port 82b of the second rotary joint 82 into the rotary container 11 via the stock solution supply passage 14a at a constant supply speed. At this time, since the first electromagnetic valve 71 is off, the high-pressure oil 40 (FIG. 2) is not supplied into the cylinder 30b, and the cylinder 30b is maintained at the highest position by the elastic force of the cylinder spring 30c. Valve seat 2 of body 29
9a comes into close contact with the crystal outlet 14d and closes the crystal outlet 14d. In addition, since the valve body 29 rotates together with the rotating container 11, the centrifugal force generated in the weight 29b urges the valve body 29 to rotate in the direction of the dashed arrow in FIG. As a result, the adhesion of the valve seat 29a to the crystal outlet 11d is improved. The nitric acid solution 17 sequentially supplied into the rotating container 11 is cooled by a cooling liquid to precipitate nitric acid compound crystals 17b.
Is deposited on the inner surface of the outermost peripheral portion of the rotating container 11 by the centrifugal force caused by the rotation of the rotating container 11. The mother liquor 17a of the nitric acid solution 17 in the rotating container 11 is supplied to the mother liquor outlet 1 via a mother liquor discharge passage 13a, a mother liquor discharge pipe 18g, and a mother liquor discharge chamber 18c.
8e.
【0020】所定時間経過後、モータ26によるシャフ
ト12及び回転容器11の回転を停止し、同時に第2電
磁バルブ92をオフして回転容器11内の硝酸溶液17
の母液17aを原液供給通路14aを介して原液供給口
82bから排出する。次にシャフト12及び回転容器1
1を再び回転させ、第1電磁バルブ71をオンして高圧
油40を油通路13cを介してシリンダ30b内に供給
する。シリンダ30b内への高圧油40の供給により、
シリンダ30bがシリンダ用ばね30cの弾性力に抗し
て下降すると、弁座部29aが結晶出口11dから離脱
する方向に弁本体29が回転して図2に示す位置に至
り、この開放された結晶出口11dから硝酸化合物結晶
17bが回転容器11の回転による遠心力にて結晶排出
室18dに排出され、更に結晶排出口18fから排出さ
れる。回転容器11からの結晶17bの排出が終了する
と、第1電磁バルブ71はオフして弁座部29aにより
結晶出口11dを閉止し、第2電磁バルブ92をオンし
て硝酸溶液17を回転容器11内に供給して、上記動作
を繰返す。このように硝酸溶液17の冷却晶析と固液分
離を同時にかつ短時間で効率よく行うことができる。After a lapse of a predetermined time, the rotation of the shaft 12 and the rotary container 11 by the motor 26 is stopped, and at the same time, the second electromagnetic valve 92 is turned off to turn off the nitric acid solution 17 in the rotary container 11.
Is discharged from the stock solution supply port 82b through the stock solution supply passage 14a. Next, the shaft 12 and the rotating container 1
1 is rotated again, the first electromagnetic valve 71 is turned on, and the high-pressure oil 40 is supplied into the cylinder 30b via the oil passage 13c. By supplying the high-pressure oil 40 into the cylinder 30b,
When the cylinder 30b descends against the elastic force of the cylinder spring 30c, the valve body 29 rotates in the direction in which the valve seat portion 29a separates from the crystal outlet 11d to reach the position shown in FIG. The nitrate compound crystal 17b is discharged from the outlet 11d into the crystal discharge chamber 18d by centrifugal force generated by the rotation of the rotary container 11, and further discharged from the crystal discharge port 18f. When the discharge of the crystal 17b from the rotating container 11 is completed, the first electromagnetic valve 71 is turned off, the crystal outlet 11d is closed by the valve seat 29a, and the second electromagnetic valve 92 is turned on to transfer the nitric acid solution 17 to the rotating container 11 And the above operation is repeated. In this manner, the cooling crystallization and the solid-liquid separation of the nitric acid solution 17 can be performed simultaneously and efficiently in a short time.
【0021】[0021]
【発明の効果】以上述べたように、本発明によれば、硝
酸溶液を貯留可能な回転容器をアッパコーン及びロアコ
ーン互いに接合することにより形成し、この回転容器を
鉛直方向に延びるシャフトを中心に回転可能に構成し、
アッパコーンの周壁内部からロアコーンの周壁内部にか
けて冷却液通路を形成し、更に回転容器の最外周部に形
成された結晶出口を弁開閉機構により開放可能に閉止し
たので、回転容器を回転させかつ冷却液通路に冷却液を
供給しながら、回転容器に硝酸溶液を供給すると、この
硝酸溶液が冷却液により冷却されて硝酸化合物結晶が析
出し、この結晶が回転容器の回転による遠心力にて回転
容器の最外周部内面に堆積する。次に回転容器を停止し
て回転容器内の硝酸溶液の母液を排出した後、再び回転
容器を回転させ、弁開閉機構により結晶出口を開放する
と、上記結晶は遠心力により結晶出口から回転容器外に
排出される。このように短時間でかつ同時に硝酸溶液の
冷却晶析と固液分離を行うことができる。As described above, according to the present invention, a rotating container capable of storing a nitric acid solution is formed by joining an upper cone and a lower cone to each other, and the rotating container is rotated about a shaft extending in a vertical direction. Configure as possible,
A cooling liquid passage was formed from the inner wall of the upper cone to the inner wall of the lower cone, and the crystal outlet formed at the outermost periphery of the rotating container was closed by a valve opening / closing mechanism so as to be openable. When the nitric acid solution is supplied to the rotating container while supplying the cooling liquid to the passage, the nitric acid solution is cooled by the cooling liquid to precipitate a nitrate compound crystal, and the crystal is centrifugally generated by the rotation of the rotating container to rotate the rotating container. It is deposited on the inner surface of the outermost periphery. Next, after stopping the rotating container and discharging the mother liquor of the nitric acid solution in the rotating container, the rotating container is rotated again, and the crystal outlet is opened by the valve opening / closing mechanism. Is discharged. Thus, the cooling crystallization and the solid-liquid separation of the nitric acid solution can be performed in a short time and simultaneously.
【0022】また装置が大型化する従来の晶析装置と比
較して、本発明では上記のように同時に硝酸溶液の冷却
晶析と固液分離を行うことができるので、冷却晶析及び
固液分離のプロセスを大幅にコンパクト化できる。弁開
閉機構の弁本体の略中央を回転容器に支持ピンを介して
枢着し、弁本体の先端に回転容器の結晶出口に密着する
弁座部を設け、弁本体の基端に弁座部を結晶出口に密着
又は結晶出口から離脱させる弁本体駆動手段を連結し、
弁本体にウエイトを設ければ、弁開閉機構により結晶出
口が閉止され、かつ弁本体が回転容器とともに回転する
ときに、ウエイトに発生する遠心力により弁座部が結晶
出口に密着する方向に弁本体が付勢されるので、弁座部
の結晶出口への密着性が向上する。Further, in comparison with the conventional crystallization apparatus in which the size of the apparatus is increased, in the present invention, the cooling crystallization and the solid-liquid separation of the nitric acid solution can be simultaneously performed as described above. The separation process can be made much more compact. A substantially center of the valve body of the valve opening / closing mechanism is pivotally connected to the rotary container via a support pin, and a valve seat portion is provided at the tip of the valve body so as to be in close contact with the crystal outlet of the rotary container. Connect the valve body drive means to close the crystal outlet or detach from the crystal outlet,
If a weight is provided on the valve body, the crystal outlet is closed by the valve opening / closing mechanism, and when the valve body rotates together with the rotary container, the valve seat is brought into close contact with the crystal outlet due to centrifugal force generated in the weight. Since the main body is urged, the adhesion of the valve seat to the crystal outlet is improved.
【図面の簡単な説明】[Brief description of the drawings]
【図1】本発明一実施形態の晶析・分離装置の断面図。FIG. 1 is a sectional view of a crystallization / separation apparatus according to an embodiment of the present invention.
【図2】その装置の弁開閉機構により結晶出口を開放し
た状態を示す図1に対応する断面図。FIG. 2 is a sectional view corresponding to FIG. 1 and showing a state in which a crystal outlet is opened by a valve opening / closing mechanism of the apparatus.
【図3】図1のA部拡大断面図。FIG. 3 is an enlarged sectional view of a portion A in FIG. 1;
【図4】図1のB部拡大断面図。FIG. 4 is an enlarged sectional view of a portion B in FIG. 1;
10 晶析・分離装置 11 回転容器 11a アッパコーン 11b ロアコーン 11c 冷却液通路 11d 結晶出口 11e,11f 末広開口部 12 シャフト 16 弁開閉機構 17 硝酸溶液 17b 硝酸化合物結晶 29 弁本体 29a 弁座部 29b ウエイト 29d 支持ピン 30 弁本体駆動手段 DESCRIPTION OF SYMBOLS 10 Crystallization / separation apparatus 11 Rotating container 11a Upper cone 11b Lower cone 11c Coolant passage 11d Crystal outlet 11e, 11f Spherical opening 12 Shaft 16 Valve opening / closing mechanism 17 Nitric acid solution 17b Nitric acid compound crystal 29 Valve body 29a Valve seat 29b Weight 29d Support Pin 30 Valve body driving means
───────────────────────────────────────────────────── フロントページの続き (72)発明者 西村 建二 茨城県那珂郡那珂町大字向山字六人頭 1002番地の14 三菱マテリアル株式会社 那珂エネルギー研究所内 (56)参考文献 特開 昭64−85153(JP,A) 実開 昭64−48102(JP,U) (58)調査した分野(Int.Cl.7,DB名) G21C 19/46 G21F 9/06 ────────────────────────────────────────────────── ─── Continuing from the front page (72) Inventor Kenji Nishimura, Naka-cho, Naka-machi, Naka-gun, Ibaraki Pref. 1002, 1414 Mitsubishi Materials Corporation Naka Energy Laboratory (56) References JP-A-64-85153 (JP, A) Japanese Utility Model Showa 64-48102 (JP, U) (58) Fields investigated (Int. Cl. 7 , DB name) G21C 19/46 G21F 9/06
Claims (2)
硝酸溶液(17)、或いはピューレックス溶媒抽出プロセス
において共除染・分配工程から得られるU或いはPuを
含む硝酸溶液(17)を冷却して硝酸化合物結晶(17b)を析
出させ前記硝酸化合物結晶(17b)を含むスラリーから前
記硝酸化合物結晶(17b)を分離する晶析・分離装置にお
いて、 下端に末広開口部(11e)が形成されたアッパコーン(11a)
と上端に末広開口部(11f)が形成されたロアコーン(11b)
とを有し前記各末広開口部(11e,11f)の周縁を互いに接
合することにより内部に前記硝酸溶液(17)を貯留可能に
形成されかつ前記アッパコーン(11a)の上端及び前記ロ
アコーン(11b)の下端に鉛直方向に延びて接続されたシ
ャフト(12)を中心に回転可能な回転容器(11)と、 前記アッパコーン(11a)の周壁内部から前記ロアコーン
(11b)の周壁内部にかけて形成され前記回転容器(11)内
の前記硝酸溶液(17)を冷却して硝酸化合物結晶(17b)を
析出する冷却液が通過可能な冷却液通路(11c)と、 前記回転容器(11)の最外周部に形成され前記回転容器(1
1)の回転による遠心力にて前記最外周部内面に堆積した
前記硝酸化合物結晶(17b)を排出可能な結晶出口(11d)
と、 前記結晶出口(11d)を開放可能に閉止する弁開閉機構(1
6)とを備えたことを特徴とする晶析・分離装置。1. Cooling a nitric acid solution (17) containing U and Pu in which spent nuclear fuel is dissolved, or a nitric acid solution (17) containing U or Pu obtained from a co-decontamination and distribution step in a purex solvent extraction process. In the crystallization / separation apparatus for separating the nitrate compound crystal (17b) from the slurry containing the nitrate compound crystal (17b) by depositing the nitrate compound crystal (17b), a divergent opening (11e) is formed at the lower end. Ta upper cone (11a)
And a lower cone (11b) with a divergent opening (11f) at the upper end
By joining the peripheral edges of the divergent openings (11e, 11f) to each other, the nitric acid solution (17) is formed therein so as to be able to store therein, and the upper end of the upper cone (11a) and the lower cone (11b) are formed. A rotatable container (11) rotatable around a shaft (12) extending vertically and connected to the lower end of the lower cone, and the lower cone from inside the peripheral wall of the upper cone (11a).
A cooling liquid passageway (11c) formed around the inside of the peripheral wall of (11b) and through which a cooling liquid for cooling the nitric acid solution (17) in the rotating container (11) to precipitate a nitrate compound crystal (17b) can pass; The rotating container (1) formed at the outermost peripheral portion of the rotating container (11)
A crystal outlet (11d) capable of discharging the nitrate compound crystal (17b) deposited on the inner surface of the outermost peripheral portion by centrifugal force due to the rotation of 1)
A valve opening / closing mechanism (1) for opening and closing the crystal outlet (11d).
6) A crystallization / separation device comprising:
ピン(29d)を介して略中央が枢着された弁本体(29)と、 前記弁本体(29)の先端に形成され前記回転容器(11)の結
晶出口(11d)に密着可能な弁座部(29a)と、 前記弁本体(29)の基端に連結され前記支持ピン(29d)を
中心に前記弁本体(29)を揺動することにより前記弁座部
(29a)を前記結晶出口(11d)に密着又は前記結晶出口(11
d)から離脱させる弁本体駆動手段(30)と、 前記弁本体(29)のうちこの弁本体(29)の基端と前記支持
ピン(29d)との間に設けられ前記弁本体(29)が前記回転
容器(11)とともに回転するときに発生する遠心力により
前記弁座部(29a)が前記結晶出口(11d)に密着する方向に
前記弁本体(29)を付勢するウエイト(29b)とを備えた請
求項1記載の晶析・分離装置。2. A valve opening / closing mechanism (16) comprising: a valve body (29) pivotally connected at a substantially center to a rotary container (11) via a support pin (29d); and a tip of the valve body (29). A valve seat (29a) formed and capable of closely contacting a crystal outlet (11d) of the rotary container (11); and the valve body connected to a base end of the valve body (29) and centering on the support pin (29d). By swinging (29), the valve seat
(29a) in close contact with the crystal outlet (11d) or the crystal outlet (11
d) a valve body driving means (30) to be disengaged from the valve body (29), provided between the base end of the valve body (29) and the support pin (29d) of the valve body (29). A weight (29b) for urging the valve body (29) in a direction in which the valve seat portion (29a) comes into close contact with the crystal outlet (11d) due to centrifugal force generated when the rotary container (11) rotates with the rotating container (11). The crystallization / separation apparatus according to claim 1, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7597497A JP3143866B2 (en) | 1997-03-27 | 1997-03-27 | Crystallization / separation equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7597497A JP3143866B2 (en) | 1997-03-27 | 1997-03-27 | Crystallization / separation equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH10268091A JPH10268091A (en) | 1998-10-09 |
| JP3143866B2 true JP3143866B2 (en) | 2001-03-07 |
Family
ID=13591735
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7597497A Expired - Lifetime JP3143866B2 (en) | 1997-03-27 | 1997-03-27 | Crystallization / separation equipment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3143866B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4407416B2 (en) * | 2003-07-31 | 2010-02-03 | 国立大学法人京都大学 | Precipitation method |
| JP6829457B2 (en) * | 2016-08-23 | 2021-02-10 | 国立研究開発法人日本原子力研究開発機構 | Centrifugal extractor |
| CN111870993B (en) * | 2020-09-16 | 2021-12-03 | 安徽华馨生物科技有限公司 | Production crystallization device of menthol |
| CN117462989B (en) * | 2023-12-28 | 2024-03-01 | 山西铱倍力科技有限公司 | Crystallization equipment is used in chloroiridium acid production |
-
1997
- 1997-03-27 JP JP7597497A patent/JP3143866B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH10268091A (en) | 1998-10-09 |
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