JPH082402B2 - Pressure crystallization separation equipment and pressure crystallization separation method - Google Patents
Pressure crystallization separation equipment and pressure crystallization separation methodInfo
- Publication number
- JPH082402B2 JPH082402B2 JP63035824A JP3582488A JPH082402B2 JP H082402 B2 JPH082402 B2 JP H082402B2 JP 63035824 A JP63035824 A JP 63035824A JP 3582488 A JP3582488 A JP 3582488A JP H082402 B2 JPH082402 B2 JP H082402B2
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- material liquid
- pressure
- pressure crystallization
- heat
- 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 - Fee Related
Links
- 238000002425 crystallisation Methods 0.000 title claims description 152
- 230000008025 crystallization Effects 0.000 title claims description 147
- 238000000926 separation method Methods 0.000 title claims description 78
- 239000007788 liquid Substances 0.000 claims description 157
- 239000002994 raw material Substances 0.000 claims description 150
- 238000001816 cooling Methods 0.000 claims description 28
- 239000013078 crystal Substances 0.000 claims description 17
- 239000002002 slurry Substances 0.000 description 23
- 239000000047 product Substances 0.000 description 17
- 238000000034 method Methods 0.000 description 12
- 238000007711 solidification Methods 0.000 description 11
- 230000008023 solidification Effects 0.000 description 11
- 239000007791 liquid phase Substances 0.000 description 8
- 238000004781 supercooling Methods 0.000 description 8
- 229910000831 Steel Inorganic materials 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000010959 steel Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 239000012265 solid product Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229930003836 cresol Natural products 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- RLSSMJSEOOYNOY-UHFFFAOYSA-N m-cresol Chemical compound CC1=CC=CC(O)=C1 RLSSMJSEOOYNOY-UHFFFAOYSA-N 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000011265 semifinished product Substances 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 208000019014 inability to feed Diseases 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 230000035900 sweating Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は、圧力晶析用原料液を温度調整して圧力晶析
分離装置へ供給し、断熱的な加圧固化、減圧融解及び固
液分離操作を組み合わせて行い、該原料液から目的成分
のみを分離精製する圧力晶析分離設備及び圧力晶析分離
方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial field of application) The present invention relates to the adiabatic pressure solidification, reduced pressure melting and solid-liquid reaction of a pressure crystallization raw material liquid that is temperature-controlled and supplied to a pressure crystallization separator. The present invention relates to a pressure crystallization separation facility and a pressure crystallization separation method for separating and purifying only a target component from the raw material liquid by performing a combination of separation operations.
（従来の技術） 圧力晶析法は、従来の蒸留法や冷却晶析法では分離困
難な原料系への適用に大きな可能性を有している事、高
純度の製品が得易い事、高収率が得られる事及びエネル
ギ消費量が少ない事から、近年の化学工場のファイン化
に伴って大きな注目を集めている分離精製技術である。(Prior Art) The pressure crystallization method has great potential for application to a raw material system that is difficult to separate by the conventional distillation method or cooling crystallization method, that a high-purity product is easily obtained, and It is a separation and purification technology that has been attracting a great deal of attention with the recent refinement of chemical factories because it can obtain a yield and consumes less energy.
かかる圧力晶析法の概要は、冷えば、化学工業Vol.5
0,No.5,P331−335「圧力晶析法と装置の概要」に記載さ
れている。これを第３図（プロセスフロー図）によって
説明すると、圧力容器（１）には、下方に蓋体（下蓋）
（２）が設けられ、ピストン（５）が油圧ユニット
（３）の作動により容器（１）内で上下動するように設
けられ、このピストン（５）の下蓋（２）とによって圧
力容器（１）内に晶析室（４）が形成される。この晶析
室（４）と排液タンク（６）とが、減圧機構（10）及び
弁（11）を介して配管（９）により連結されている。
又、晶析室（４）と予備晶析缶（７）とが原料供給ポン
プ（８）、弁（12）を介して配管（13）により連結され
ている。The outline of this pressure crystallization method is as follows.
0, No. 5, P331-335 "Outline of Pressure Crystallization Method and Equipment". This will be described with reference to FIG. 3 (process flow diagram). In the pressure vessel (1), a lid (lower lid) is provided below.
(2) is provided, and the piston (5) is provided so as to move up and down in the container (1) by the operation of the hydraulic unit (3). A crystallization chamber (4) is formed in 1). The crystallization chamber (4) and the drainage tank (6) are connected by a pipe (9) via a pressure reducing mechanism (10) and a valve (11).
Further, the crystallization chamber (4) and the preliminary crystallization can (7) are connected by a pipe (13) via a raw material supply pump (8) and a valve (12).
この設備において、原料は原料タンク（14）より予備
晶析缶（７）に送給されて圧力晶析のための種結晶を生
成する。これは種結晶を含まないままの原料を圧力晶析
にかけると、圧力晶析では過飽和圧が一般的に数百気圧
以上と比較的高い場合が多く、初期結晶生成の為に高圧
力が必要となる恐れがあるためであり、種結晶を含んだ
スラリ状態で給液すると、かかる過飽和圧の心配がない
ばかりか加圧により核発生を伴わずに結晶の成長が期待
出来る利点がある。In this facility, the raw material is fed from the raw material tank (14) to the preliminary crystallization can (7) to generate seed crystals for pressure crystallization. This is because when the raw material without containing seed crystals is subjected to pressure crystallization, the supersaturation pressure in pressure crystallization is generally relatively high, at several hundred atmospheres or higher, and high pressure is required for initial crystal formation. When the liquid is supplied in a slurry state containing seed crystals, there is an advantage that not only there is no concern about such supersaturation pressure, but also crystal growth can be expected without generation of nuclei by pressurization.
次に、配管（13）から弁（12）を介して原料を晶析室
（４）に注入する。晶析室（４）内に原料が充満する
と、ピストン先端部に開口を有するオーバーフロー管
（15）を通って液流出が始まるので、これを検知して弁
（12），（16）を閉じてピストン（５）による加圧を開
始する。原料液を加圧すると原料中の特定物質の結晶化
が進行して、晶析室（４）内は高圧下の固液平衡状態と
なる。このとき生成する固体は一般に極めて高純度の物
質である。尚、固化の進行に伴って発生する固化潜熱に
より、晶析室（４）内の温度は上昇するが、圧力晶析法
では一般にこの温度上昇防止の為の冷却は行わず、断面
的に加圧する方法が採用される。昇温後の到達温度即ち
固液分離開始温度は、製品の純度、収率に影響を及ぼす
から、これは原料混合物の比熱、固化潜熱等を考慮して
給液温度により調整する。Next, the raw material is injected into the crystallization chamber (4) from the pipe (13) through the valve (12). When the crystallization chamber (4) is filled with the raw material, the liquid begins to flow out through the overflow pipe (15) having an opening at the tip of the piston. When this is detected, the valves (12) and (16) are closed. Pressurization by the piston (5) is started. When the raw material liquid is pressurized, crystallization of the specific substance in the raw material proceeds, and the inside of the crystallization chamber (4) is in a solid-liquid equilibrium state under high pressure. The solid formed at this time is generally an extremely high-purity substance. The temperature in the crystallization chamber (4) rises due to the latent heat of solidification generated with the progress of solidification, but in the pressure crystallization method, cooling is generally not performed to prevent this temperature rise, and cross-section is applied. The method of pressing is adopted. The temperature reached after the temperature is raised, that is, the solid-liquid separation start temperature affects the purity and yield of the product. Therefore, this is adjusted by the liquid supply temperature in consideration of the specific heat of the raw material mixture, the latent heat of solidification and the like.
次に、所定の圧力まで昇圧し、所定の固液比率に達す
ると、油圧ユニット（３）からピストン（５）に作用す
る圧力を保持して晶析室（４）内の圧力を保持したまま
ピストンの下降を続けると、晶析室（４）内の結晶粒群
は加圧圧搾され、結晶粒間の残留液体は所謂「絞り出し
作用」を受けて排液タンク（６）に排出される。Next, when the pressure is increased to a predetermined pressure and a predetermined solid-liquid ratio is reached, the pressure acting on the piston (5) from the hydraulic unit (3) is maintained and the pressure in the crystallization chamber (4) is maintained. When the piston continues to descend, the crystal grain group in the crystallization chamber (4) is compressed under pressure, and the residual liquid between the crystal grains undergoes a so-called "squeeze action" and is discharged to the drainage tank (6).
ピストン（５）の下降がさらに続くと、結晶粒群は晶
析室（４）の形状に沿って一個の大きな塊状固体製品へ
と成形されていく。このようにして液体を固体から略完
全に分離する段階になると、大気圧下の排液タンク
（６）に連通している晶析室（４）内の液相圧力は次第
に低下していくため、結晶表面は部分的に融解し、所謂
「発汗洗浄」が行われ塊状固体製品の精製がなされる。When the piston (5) is further lowered, the crystal grains are formed into one large lump solid product along the shape of the crystallization chamber (4). In this way, when the liquid is almost completely separated from the solid, the liquid phase pressure in the crystallization chamber (4) communicating with the drainage tank (6) under atmospheric pressure gradually decreases. The crystal surface is partially melted, and so-called "perspiration cleaning" is performed to purify the solid solid product.
晶析室（４）から排出される排液の圧力が所定の圧力
まで低下すると、ピストン（５）の下降を停止し、同ピ
ストンの上昇を開始すると共に高圧容器（１）も上昇さ
せると、固体製品は下蓋（２）上に載置された状態で容
器（１）から取り出される。これを製品取り出し装置
（図示せず）によって取り出し、高圧容器（１）を下降
させて下蓋（２）に装着し、以下原料の注入工程に戻
り、同様の工程を繰り返す事になる。尚、原料の注入に
先立ち、前述のオーバーフロー管（15）内の残液を、窒
素ガスでパージし、次工程の注入時の満液検知の為の準
備をしておく。When the pressure of the waste liquid discharged from the crystallization chamber (4) decreases to a predetermined pressure, the lowering of the piston (5) is stopped, the ascending of the piston is started, and the high pressure container (1) is also raised. The solid product is taken out of the container (1) while being placed on the lower lid (2). This is taken out by a product take-out device (not shown), the high-pressure container (1) is lowered and attached to the lower lid (2), and then the process of injecting the raw material is repeated and the same process is repeated. Prior to the injection of the raw material, the above-mentioned residual liquid in the overflow pipe (15) is purged with nitrogen gas to prepare for full liquid detection at the time of injection in the next step.
以上の如く、従来の圧力晶析分離設備は、予備晶析缶
（以降、予冷槽という）と、ポンプと、圧力晶析分離装
置とがこの順に管接続されたものである。As described above, in the conventional pressure crystallization separation equipment, a preliminary crystallization can (hereinafter referred to as a precooling tank), a pump, and a pressure crystallization separation device are connected in this order by pipes.
そして圧力晶析分離は、前記予冷槽により原料液を圧
力晶析分離に必要な温度（T0）に予冷却した後、ポンプ
により圧力晶析分離装置へ供給し、該装置により断熱的
な加圧固化、減圧融解および固液分離操作を繰り返して
行うものである。In the pressure crystallization separation, the raw material liquid is precooled to the temperature (T 0 ) required for pressure crystallization separation by the precooling tank, and then supplied to the pressure crystallization separation device by a pump, and the device is adiabatically applied. This is repeated pressure solidification, melting under reduced pressure and solid-liquid separation.
上記原料液の予冷却は、圧力晶析時の種結晶を生じさ
せるために行われるものであるので、予冷却後の原料液
は、固液共存状態のスラリ液となっている。尚、原料液
の固相濃度は、高い程収率が高くなるが、原料液の送給
がし難くなるので、ポンプの送給能力、特にポンプ吸い
込み側能力との関係により、制限される。例えば、固相
濃度が20乃至25％程度のスラリ液となっている。Since the pre-cooling of the raw material liquid is performed in order to generate seed crystals during pressure crystallization, the raw material liquid after pre-cooling is a slurry liquid in a solid-liquid coexisting state. Although the higher the solid phase concentration of the raw material liquid, the higher the yield, the more difficult it becomes to feed the raw material liquid. Therefore, the solid-state concentration is limited by the feed ability of the pump, particularly the pump suction side ability. For example, the slurry liquid has a solid phase concentration of about 20 to 25%.
上記原料液の種結晶の状態は、分離精製する目的成分
（目的製品）の純度、収率を決定する主要因であり、原
料液の温度と密接な関係がある。従って、上記圧力晶析
分離装置の圧力晶析室へ供給される原料液の温度条件
は、主に目的製品に対応して定められ、圧力晶析室での
原料液の温度を所定の温度（T0）に制御することは極め
て重要である。同様に、給液後の加圧晶析操作、液相成
分の分離排出操作、減圧発汗操作においても、各操作に
伴って断熱的に変化する晶析室内の温度を維持すること
も極めて重要である。そこで圧力晶析分離装置は、次の
ような断熱的対策が採られている。第２図に断熱的対策
が採られた圧力晶析分離装置の概念を示す。この装置
は、厚肉鋼製高圧容器の胴部（17）、下蓋部（18）およ
びピストン（19）等からなり、胴部（17）内面、フィル
タ（21）背面等の高圧容器内面の一部又は全部に断熱材
（23）が断熱支持材（26）により支持されて設けられ、
更に断熱効果の助長手段、例えばヒータ（24）等が設け
られている。これは、高圧容器内原料又は半製品と厚肉
鋼製高圧容器との熱交換を抑制し、また、原料又は半製
品の温度が不均一になることを避けるためである。高圧
容器の温度は、既に述べた通り変化する晶析室（25）内
スラリ液の時間平均値に調整される。The state of the seed crystals of the raw material liquid is a main factor that determines the purity and yield of the target component (target product) to be separated and purified, and is closely related to the temperature of the raw material liquid. Therefore, the temperature condition of the raw material liquid supplied to the pressure crystallization chamber of the pressure crystallization separator is determined mainly in accordance with the target product, and the temperature of the raw material liquid in the pressure crystallization chamber is set to a predetermined temperature ( Controlling to T 0 ) is extremely important. Similarly, it is also extremely important to maintain the temperature inside the crystallization chamber, which changes adiabatically with each operation, even in the pressure crystallization operation after the liquid supply, the separation and discharge operation of the liquid phase components, and the reduced pressure perspiration operation. is there. Therefore, the pressure crystallization separator has the following adiabatic measures. Fig. 2 shows the concept of a pressure crystallization separator with adiabatic measures. This device is composed of the body (17) of the thick-walled steel high-pressure container, the lower lid (18), the piston (19), etc., and the inner surface of the body (17), the back surface of the filter (21), etc. A heat insulating material (23) is provided partially or entirely by being supported by a heat insulating support material (26),
Further, a means for promoting the heat insulation effect, such as a heater (24), is provided. This is to suppress heat exchange between the raw material or semi-finished product in the high-pressure container and the high-pressure vessel made of thick-walled steel, and to prevent the temperature of the raw material or semi-finished product from becoming non-uniform. The temperature of the high-pressure vessel is adjusted to the time average value of the slurry liquid in the crystallization chamber (25) which changes as described above.
（発明が解決しようとする課題） ところが、上記断熱材（23）の効果は、原料液が圧力
晶析分離装置の晶析室（25）へ供給された後に発揮され
るものであり、断熱材の使用が困難な圧力晶析分離装置
の厚肉鋼製高圧容器壁内に位置する原料液供給用配管
（22）部分では、高圧容器壁と原料液との温度差により
配管を介して両者の間で熱交換が行われる。従って、原
料液を予冷却して圧力晶析分離に必要な温度（T0）にす
るだけでは、原料液が晶析室へ供給された時、圧力晶析
分離に必要な温度（T0）より高い温度（T1）に上昇して
いるという問題点がある。この温度上昇は目的製品の収
率の低下を招くことに繋がる。一方、高圧容器の温度を
圧力晶析分離に必要な温度（T0）に調整することは、液
相分の排出工程において、排出液が冷却され、液相分の
排出配管内において結晶が析出して閉塞するという新た
な問題点が生じる。(Problems to be Solved by the Invention) However, the effect of the heat insulating material (23) is exhibited after the raw material liquid is supplied to the crystallization chamber (25) of the pressure crystallization separator. It is difficult to use the pressure crystallization separation device in the thick-walled steel high-pressure vessel wall where the raw material liquid supply pipe (22) is located. Heat exchange takes place between them. Thus, raw material solution was precooled only to a temperature (T 0) required for the pressure crystallization separation, when the raw material liquid is supplied to the crystallization chamber, required pressure crystallization separation temperature (T 0) There is a problem that the temperature is rising to a higher temperature (T 1 ). This increase in temperature leads to a decrease in the yield of the target product. On the other hand, adjusting the temperature of the high-pressure vessel to the temperature (T 0 ) required for pressure crystallization separation causes the discharged liquid to be cooled in the liquid phase discharging process and crystals to precipitate in the liquid phase discharging pipe. Then, a new problem arises that it is blocked.
原料液が晶析室（25）へ供給された時温度が上昇する
という問題点に対する対策として、予冷槽で原料液を圧
力晶析分離に必要な温度（T0）よりも低い温度（T2）に
過冷却しておく方法が考えられる。しかし、この方法
は、極めて困難な予冷操作を更に困難なものとし、また
予冷槽の能力増強を必要とし、これに対応して予冷槽の
装置費の増加を招くという問題点がある。また、過冷却
により原料液中の固相濃度（以降、スラリ濃度という）
が高くなるので、スラリ濃度がポンプ吸い込み側能力に
より定まるスラリ濃度の制限値以上となることがあり、
この場合は原料液の送給ができなくなるという問題点が
ある。また、このとき、元の原料液中の成分濃度を低
め、過冷却後のスラリ濃度を前記ポンプによるスラリ濃
度の制限値以下になるようにすれば、原料液送給を可能
とすることができるが、その場合はやはり目的製品の収
率の低下を招くという問題点がある。As a countermeasure against the problem that the temperature rises when the raw material liquid is supplied to the crystallization chamber (25), a temperature lower than the temperature (T 0) required pressure crystallization separating material solution in the pre-cooling tank (T 2 ) Is considered to be supercooled. However, this method has a problem that the extremely difficult precooling operation is made more difficult, and the capacity of the precooling tank is required to be increased, and correspondingly, the apparatus cost of the precooling tank is increased. Also, the solid phase concentration in the raw material liquid due to supercooling (hereinafter referred to as slurry concentration)
, The slurry concentration may exceed the limit value of the slurry concentration determined by the pump suction side capacity.
In this case, there is a problem that the raw material liquid cannot be fed. Further, at this time, if the component concentration in the original raw material liquid is lowered so that the slurry concentration after supercooling is equal to or less than the limit value of the slurry concentration by the pump, the raw material liquid can be fed. However, in that case, there is still a problem that the yield of the target product is lowered.
本発明はこの様な事情に着目してなされたものであっ
て、その目的は従来のものがもつ以上のような問題点を
解消し、予冷槽での原料液の過冷却をすることなく、ま
た、元の原料液中の成分濃度を低めることなく、予冷槽
により予冷却されて圧力晶析分離に必要な所定温度
（T0）に調整された原料液（スラリ液）が圧力晶析分離
装置の晶析室へ供給され、到達した時の原料液の温度を
圧力晶析分離に必要な温度（T0）にでき、そのために予
冷操作の困難化、予冷槽の能力増強、原料液の送給不可
を招くことなく、目的製品収率の向上が図れる圧力晶析
分離設備および圧力晶析分離方法を提供しようとするも
のである。The present invention has been made by paying attention to such a situation, and its object is to solve the above-mentioned problems of the conventional one, without subcooling the raw material liquid in the precooling tank, In addition, the raw material liquid (slurry liquid) precooled in the precooling tank and adjusted to the predetermined temperature (T 0 ) necessary for pressure crystallization separation without lowering the concentration of the components in the original raw material liquid is pressure crystallization separated. The temperature of the raw material liquid when it is supplied to the crystallization chamber of the equipment and reaches it can be adjusted to the temperature (T 0 ) required for pressure crystallization separation, which makes the precooling operation difficult, increases the capacity of the precooling tank, An object of the present invention is to provide a pressure crystallization separation facility and a pressure crystallization separation method capable of improving the yield of a target product without inviting a feed failure.
（課題を解決するための手段） 上記の目的を達成するために、本発明は次のような構
成の圧力晶析分離設備および圧力晶析分離方法としてい
る。(Means for Solving the Problems) In order to achieve the above object, the present invention provides a pressure crystallization separation facility and a pressure crystallization separation method having the following configurations.
即ち、本発明は、圧力晶析分離用原料液の予冷槽と、
原料液を予冷槽から圧力晶析分離装置へ送給するポンプ
と、送給された原料液の圧力晶析分離を行う圧力晶析分
離装置とを有する圧力晶析分離設備において、前記ポン
プと前記圧力晶析分離装置との間に、冷却用熱媒槽及び
保温用熱媒槽を付帯した熱交換器を接続してなることを
特徴とする圧力晶析分離設備である。That is, the present invention, a pre-cooling tank of the raw material liquid for pressure crystallization separation,
A pump for feeding a raw material liquid from a precooling tank to a pressure crystallization separation device, and a pressure crystallization separation device having a pressure crystallization separation device for performing pressure crystallization separation of the fed raw material liquid, wherein the pump and the The pressure crystallization separation apparatus is characterized in that a heat exchanger equipped with a cooling heat medium tank and a heat retention heat medium tank is connected between the pressure crystallization separation apparatus.
又、圧力晶析分離に必要な温度に予冷却された原料液
を原料液送給用ポンプで圧力晶析分離装置へ供給し、圧
力晶析分離することを繰り返して行う圧力晶析分離方法
において、前記圧力晶析分離装置への原料液供給の間、
前記予冷却された原料液から、原料液が圧力晶析分離装
置の高圧容器壁内に位置する原料液供給用配管内を通過
する際に高圧容器壁から受ける入熱量に相当する熱量
を、原料液送給用ポンプと圧力晶析分離装置との間で、
この間に接続した熱交換器に冷却用熱媒を導入すること
により除去しながら、圧力晶析分離装置への原料液供給
を行い、この原料液供給後から次の原料液供給開始前に
いたる原料液供給停止の間、上記熱交換器に保温用熱媒
を導入することを特徴とする圧力晶析分離方法である。Further, in a pressure crystallization separation method in which a raw material liquid precooled to a temperature required for pressure crystallization separation is supplied to a pressure crystallization separation device by a raw material liquid feed pump, and pressure crystallization separation is repeated. During the supply of the raw material liquid to the pressure crystallization separator,
From the precooled raw material liquid, the amount of heat equivalent to the heat input amount received from the high pressure vessel wall when the raw material liquid passes through the raw material liquid supply pipe located in the high pressure vessel wall of the pressure crystallization separator is Between the liquid feed pump and the pressure crystallization separator,
The raw material liquid is supplied to the pressure crystallization separator while removing it by introducing the heating medium for cooling into the heat exchanger connected during this period. The pressure crystallization separation method is characterized in that a heat-retaining heat medium is introduced into the heat exchanger while the liquid supply is stopped.
（作 用） 本発明の圧力晶析分離設備は、以上のような構成とし
ているので、該設備を圧力晶析分離に使用すれば、予冷
槽により圧力晶析分離用原料液が所定温度（T0）に予冷
却され、その後ポンプにより予冷槽から原料液が送給さ
れると、ポンプと圧力晶析分離装置との間に接続された
熱交換器（冷却用熱媒槽及び保温用熱媒槽を付帯した熱
交換器）に冷却用熱媒を導入（循環）することにより、
原料液から熱量が除去され、原料液は前記温度（T0）よ
りも低い温度（T3）になり、そして圧力晶析分離装置へ
供給されることになる。この原料液供給時、圧力晶析分
離装置の高圧容器壁内に位置する原料液供給用配管部分
において、原料液と高圧容器との間の温度差により配管
を介して熱交換が行われるので、原料液はその温度が前
記温度（T3）より高い温度（T4）になり、晶析室に供給
される。従って、原料液と高圧容器との間の熱交換によ
り原料液が受ける入熱量と、熱交換器で原料液から除去
される熱量とを等しくすれば、圧力晶析室に供給された
原料液の温度（T4）を所定温度（T0）に等しくし得る。(Operation) Since the pressure crystallization separation equipment of the present invention is configured as described above, when the equipment is used for pressure crystallization separation, the pressure crystallization separation raw material liquid is heated to a predetermined temperature (T When the raw material liquid is fed from the precooling tank by the pump, the heat exchanger (the cooling heat medium tank and the heat retaining heat medium connected between the pump and the pressure crystallization separator) is cooled. By introducing (circulating) the cooling heat medium into the heat exchanger equipped with the tank,
The amount of heat is removed from the raw material liquid, the raw material liquid reaches a temperature (T 3 ) lower than the temperature (T 0 ) and is supplied to the pressure crystallization separator. At the time of supplying the raw material liquid, in the raw material liquid supply pipe portion located in the high pressure vessel wall of the pressure crystallization separator, heat exchange is performed through the pipe due to the temperature difference between the raw material liquid and the high pressure vessel, The temperature of the raw material liquid becomes higher (T 4 ) than the temperature (T 3 ) and is supplied to the crystallization chamber. Therefore, if the amount of heat input to the raw material liquid by heat exchange between the raw material liquid and the high-pressure vessel is made equal to the amount of heat removed from the raw material liquid in the heat exchanger, the raw material liquid supplied to the pressure crystallization chamber will be The temperature (T 4 ) can be equal to the predetermined temperature (T 0 ).
本発明の圧力晶析分離方法は、圧力晶析分離装置への
原料液供給の間、圧力晶析分離に必要な温度（T0）に予
冷却された原料液から、前記原料液と高圧容器との間の
熱交換により原料液が受ける入熱量に相当する熱量を、
原料液送給用ポンプと圧力晶析分離装置との間で、この
間に接続した熱交換器に冷却用熱媒を導入することによ
り除去（以降、予冷却後熱量除去という）しながら、圧
力晶析分離装置への原料液供給を行うようにしている。
このように、原料液と高圧容器との間の熱交換により原
料液が受ける入熱量と、予冷却後熱量除去により原料液
から除去される熱量とを等しくなるようにしている。従
って、晶析室に供給された原料液の温度（T4）は圧力晶
析分離に必要な温度（T0）にし得る。The pressure crystallization separation method of the present invention is a method in which a raw material liquid pre-cooled to a temperature (T 0 ) required for pressure crystallization separation during the supply of the raw material liquid to the pressure crystallization separation device The amount of heat equivalent to the amount of heat input to the raw material liquid due to heat exchange between
Between the raw material liquid feed pump and the pressure crystallization separator, the pressure heat crystal is removed by introducing the cooling heat medium into the heat exchanger connected between them (hereinafter, referred to as heat removal after precooling). The raw material liquid is supplied to the deposition / separation device.
In this way, the heat input to the raw material liquid due to the heat exchange between the raw material liquid and the high-pressure container is made equal to the heat amount removed from the raw material liquid by the post-precooling heat amount removal. Therefore, the temperature (T 4 ) of the raw material liquid supplied to the crystallization chamber can be the temperature (T 0 ) required for pressure crystallization separation.
熱交換器は、前記のように、ポンプと圧力晶析分離装
置との間に接続されている。また、予冷却後熱量除去
は、ポンプと圧力晶析分離装置との間で行われる必要が
ある。この理由を、以下に説明する。The heat exchanger is connected between the pump and the pressure crystallization separator as described above. In addition, heat removal after precooling needs to be performed between the pump and the pressure crystallization separator. The reason for this will be described below.
予冷却後熱量除去された原料液は、過冷却により更に
スラリ濃度が高くなる。一方、ポンプによるスラリ濃度
の制限値はポンプの吸い込み側で定まる値であるので、
吸い込み側でこの値を越えていると、原料液の送給がで
きなくなる。従って、もしも予冷却後熱量除去が予冷槽
とポンプとの間において行われれば、過冷却によるスラ
リ濃度の上昇はポンプの吸い込み側で生じることになる
ので、そのスラリ濃度が前記制限値以上となったとき、
原料液の送給ができなくなる。故に、過冷却により更に
スラリ濃度が高くなっても、常に原料液の送給ができる
ようにするためには、過冷却によるスラリ濃度の上昇
は、ポンプの吐出側で生じさせる必要がある。また、ポ
ンプの吐出側でのスラリ濃度の上昇も送給の抵抗となる
が、それは吐出圧を増強すれば簡単に解決されるもので
ある。かかる理由から、熱交換器はポンプと圧力晶析分
離装置との間に接続され、また、予冷却後熱量除去はポ
ンプと圧力晶析分離装置との間で行われるようにしてい
るのである。The raw material liquid from which the amount of heat has been removed after precooling has a higher slurry concentration due to supercooling. On the other hand, the limit value of the slurry concentration by the pump is a value determined on the suction side of the pump,
If this value is exceeded on the suction side, the raw material liquid cannot be fed. Therefore, if heat removal after precooling is performed between the precooling tank and the pump, an increase in the slurry concentration due to supercooling will occur on the suction side of the pump, so the slurry concentration will be above the limit value. When
It becomes impossible to feed the raw material liquid. Therefore, in order to always be able to feed the raw material liquid even if the slurry concentration becomes higher due to supercooling, the increase in slurry concentration due to supercooling must be caused on the discharge side of the pump. Further, an increase in the slurry concentration on the discharge side of the pump also becomes a resistance to the feed, but this can be easily solved by increasing the discharge pressure. For this reason, the heat exchanger is connected between the pump and the pressure crystallization separator, and the post-precooling heat quantity removal is performed between the pump and the pressure crystallization separator.
尚、予冷却後熱量除去された後の原料液は、圧力晶析
時の種結晶の他に、過冷却によって新たに生じた結晶を
含有しているが、この新生結晶は前記圧力容器壁から受
ける入熱量によって再融解する性状の結晶であるので、
予冷却後熱量除去は目的製品の純度、収率に何ら影響を
及ぼすものではない。Incidentally, the raw material liquid after the heat removal after precooling contains, in addition to the seed crystal at the time of pressure crystallization, crystals newly generated by supercooling. Because it is a crystal that remelts depending on the amount of heat input it receives,
The removal of heat after precooling does not affect the purity and yield of the target product.
前記原料液の送給後は、圧力晶析分離が行われ、そし
て製品が取り出され、次工程の原料液送給のための準備
をした後、前記と同様の次の原料液送給が開始され、同
様の原料液送給（予冷却後熱量除去しながら原料液送
給）が行われる。After the feed of the raw material liquid, pressure crystallization separation is performed, the product is taken out, and preparation for the feed of the raw material liquid in the next step is performed, and then the feed of the next raw material liquid similar to the above is started. Then, the same feed of the raw material liquid (feed of the raw material liquid while removing the amount of heat after precooling) is performed.
このとき、原料液送給後、前記熱交換器に循環する熱
媒を冷却用熱媒から保温用熱媒に切り換え、次の原料液
送給開始前にいたる原料液送給停止の間、熱交換器に保
温用熱媒を導入（循環）することにより、この間におけ
る原料液送給管内の原料液の温度低下による固化を確実
に防止することができ、そのため、以降の運転の継続の
困難化や不能化等の支障を招くことなく、次の原料液送
給を円滑に行うことができる。At this time, after the feed of the raw material liquid, the heat medium circulating in the heat exchanger is switched from the heat medium for cooling to the heat medium for heat retention, and heat is supplied during the stop of the feed of the raw material liquid before the start of the next feed of the raw material liquid. By introducing (circulating) the heat-retaining heat medium into the exchanger, it is possible to reliably prevent the solidification of the raw material liquid in the raw material liquid supply pipe during this period due to temperature decrease, which makes it difficult to continue the operation thereafter. It is possible to smoothly feed the next raw material liquid without causing troubles such as disabling.
即ち、前記熱交換器は冷却用熱媒槽及び保温用熱媒槽
を付帯した熱交換器であり、熱媒槽が冷却用熱媒槽と保
温用熱媒槽とに区分されていることから、前記熱交換器
に循環する熱媒を冷却用熱媒から保温用熱媒に直ちに切
り換えることができる。そこで、原料液送給後、前記熱
交換器に循環する熱媒を冷却用熱媒から保温用熱媒に直
ちに切り換えると、原料液送給後から次の原料液送給開
始前にいたる原料液送給停止の間、熱交換器に保温用熱
媒を循環することができ、そうすると、熱交換器及びそ
の付近に位置する原料液送給管がすぐに原料液の固化防
止のための温度以上に温められて保温され、そのため、
上記原料液送給停止の間における原料液送給管内の原料
液の温度低下（原料液送給時よりも冷却されて温度が低
くなること）を防止でき、従って、上原料液送給停止の
間における原料液送給管での原料液の固化を防止でき、
また原料液の固化による原料液送給管の閉塞を防止で
き、その結果、以降の運転（次の原料液送給工程及びそ
れ以降の工程の運転）の継続が困難になったり、不能に
なったりする等の支障を生じることなく、次の原料液送
給を円滑に行うことができる。That is, the heat exchanger is a heat exchanger accompanied by a cooling heat medium tank and a heat retaining heat medium tank, and the heat medium tank is divided into a cooling heat medium tank and a heat retaining heat medium tank. The heat medium circulating in the heat exchanger can be immediately switched from the heat medium for cooling to the heat medium for heat retention. Therefore, when the heat medium circulating in the heat exchanger is immediately switched from the cooling heat medium to the heat-retaining heat medium after the raw material liquid is fed, the raw material liquid from after feeding the raw material liquid to before starting the next raw material liquid feeding While the feeding is stopped, the heat-retaining heat medium can be circulated in the heat exchanger, so that the heat-exchanger and the raw-material feed pipes located in the vicinity of the heat-exchanger are immediately above the temperature for preventing the solidification of the raw-material liquid. Is warmed and kept warm,
It is possible to prevent the temperature of the raw material liquid in the raw material liquid supply pipe from being lowered during the stop of the supply of the raw material liquid (cooling and lowering the temperature than when the raw material liquid is fed). It is possible to prevent solidification of the raw material liquid in the raw material liquid supply pipe between
Further, it is possible to prevent clogging of the raw material liquid supply pipe due to solidification of the raw material liquid, and as a result, it becomes difficult or impossible to continue the subsequent operation (the operation of the next raw material liquid feeding step and the subsequent steps). It is possible to smoothly feed the next raw material liquid without causing any troubles such as erosion.
（実施例） 本発明に係る実施例を、図を参照しながら説明する。(Example) An example according to the present invention will be described with reference to the drawings.
実施例１ 第１図に、本発明の実施例に係るプロセスフローを示
す。使用した圧力晶析分離設備は、晶析室容量1.5の
パイロットプラントであり、予冷槽（27）と、ポンプ
（28）と、熱交換器（29）と、圧力晶析分離装置（32）
とが、この順に管接続されたものである。Example 1 FIG. 1 shows a process flow according to an example of the present invention. The pressure crystallization separation equipment used was a pilot plant with a crystallization chamber capacity of 1.5, a pre-cooling tank (27), a pump (28), a heat exchanger (29), and a pressure crystallization separation device (32).
And are pipe-connected in this order.
ここで、熱交換器（29）には冷却用熱媒槽（30）およ
び保温用熱媒槽（31）が付帯しており、原料液を圧力晶
析装置に供給している間は冷却用熱媒を導入（循環）
し、原料液供給を停止している間は保温用熱媒を供給
（循環）する。熱交換器（29）は二重管型であり、1.5m
2の伝熱面積を有するものである。Here, the heat exchanger (29) is additionally provided with a cooling heat medium tank (30) and a heat retaining heat medium tank (31) for cooling while the raw material liquid is being supplied to the pressure crystallizer. Introduce heat medium (circulation)
Then, while the supply of the raw material liquid is stopped, the heat retaining heat medium is supplied (circulated). The heat exchanger (29) is a double tube type, 1.5m
It has a heat transfer area of 2 .
予冷槽（27）の容積は100であり、そして圧力晶析
装置の運転が約50回連続してできるものである。ポンプ
（２）の送給能力は最大10/minのものである。The volume of the precooling tank (27) is 100, and the pressure crystallizer can be operated about 50 times continuously. The pump (2) has a maximum delivery capacity of 10 / min.
圧力晶析分離装置（32）は、第２図に示すものと同様
であり、厚肉鋼製高圧容器の胴部（17）、下蓋部（1
8）、ピストン（19）およびフィルタ（21）等からな
り、胴部（17）内面、フィルタ（21）背面等の高圧容器
内面に断熱板（23）が設けられ、更にヒータ（24）が設
けられている。そして給液容量1.5の晶析室（25）が
形成されている。尚、第１図においてA1,A2,A3は温度測
定器である。The pressure crystallization separator (32) is similar to that shown in FIG. 2, and includes a body (17) and a lower lid (1) of a thick-walled steel high-pressure container.
8), the piston (19), the filter (21), etc., and the heat insulating plate (23) is provided on the inner surface of the high pressure container such as the inner surface of the body (17) and the back surface of the filter (21), and the heater (24) is further provided. Has been. A crystallization chamber (25) having a liquid supply capacity of 1.5 is formed. In FIG. 1, A 1 , A 2 and A 3 are temperature measuring instruments.
上記圧力晶析分離設備を用いて、Ｐ−クレゾールの成
分を80％、ｍ−クレゾールの成分を20％含む圧力晶析分
離用の原料液（異性体混合物）についてＰ−クレゾール
を目的製品とする圧力晶析分離を、下記のようにして行
った。Using the above pressure crystallization separation equipment, P-cresol is used as a target product for a raw material liquid (isomer mixture) for pressure crystallization separation containing 80% P-cresol component and 20% m-cresol component. Pressure crystallization separation was performed as follows.
先ず、過去のデータに基づき、原料液が分離装置の高
圧容器壁内、即ち下蓋部（18）に位置する原料液供給用
配管（22）内を通過する際に圧力容器壁から受ける入熱
量を求め、その入熱量として3.72Kcalの値を得た。ま
た、圧力晶析分離の最適温度を求め、それを15℃に設定
した。次に、原料液を予冷槽（１）にて15℃に予冷却し
た。予冷却後のスラリ濃度は、18.3％であった。First, based on the past data, the amount of heat input from the pressure vessel wall when the raw material fluid passes through the high pressure vessel wall of the separator, that is, the raw material solution supply pipe (22) located in the lower lid (18). Was obtained, and a value of 3.72 Kcal was obtained as the heat input amount. Also, the optimum temperature for pressure crystallization separation was determined and set to 15 ° C. Next, the raw material liquid was precooled to 15 ° C. in the precooling tank (1). The slurry concentration after precooling was 18.3%.
予冷却後、配管のバルブを開き、ポンプ（28）を作動
させるとともに、冷却用熱媒槽（30）から熱媒を熱交換
器（29）に循環して熱交換器（29）を作動させ、予冷却
された原料液を3.0/minの流速で熱交換器（29）に送
給し、熱交換器（29）を通過させながら予冷却後熱量除
去を行った。尚、除去熱量は3.72Kcalであった。また熱
量除去直後の原料液の温度は13℃であった。この温度に
おけるスラリ濃度は、27.8％となる。After precooling, open the valve of the pipe, operate the pump (28), and circulate the heat medium from the cooling heat medium tank (30) to the heat exchanger (29) to activate the heat exchanger (29). The precooled raw material liquid was fed to the heat exchanger (29) at a flow rate of 3.0 / min, and the heat quantity was removed after precooling while passing through the heat exchanger (29). The amount of heat for removal was 3.72 Kcal. The temperature of the raw material liquid was 13 ° C. immediately after removing the heat. The slurry concentration at this temperature is 27.8%.
予冷却後熱量除去された原料液は熱交換器（29）から
更に圧力晶析分離装置（32）へ供給された。晶析室（2
5）に到達したときの原料液の温度は15℃であり、予冷
却後の温度、即ち、圧力晶析分離の最適温度と同等であ
った。The raw material liquid from which the amount of heat was removed after precooling was further supplied from the heat exchanger (29) to the pressure crystallization separator (32). Crystallization chamber (2
The temperature of the raw material liquid when reaching 5) was 15 ° C, which was equivalent to the temperature after precooling, that is, the optimum temperature for pressure crystallization separation.
晶析室（25）における原料液の量が満たされた時点で
原料液の供給を停止し、ついで圧力晶析分離を行った。
この圧力晶析分離は、ピストン（19）を下降させて1500
Kg/cm2まで加圧してスラリ濃度を更に高めた後、更にピ
ストン（19）を下降させて液相成分をフィルタ（21）、
排出管路（20）を介して分離排出し、引き続いて液相に
かかる圧力を調整しながら、減圧発汗現象により生じる
液相成分の分離圧縮をして行った。この減圧発汗操作
は、液相にかかる圧力が大気圧近傍にてほぼ一定値とな
るまで継続した。圧搾のための最大差圧は600Kg/cm2と
した。かくの如き圧力晶析分離の結果、目的製品とする
Ｐ−クレゾールが649gr得られた。その収率は、43.3％
であり、下記比較例１での収率に比較して極めて高いも
のであった。尚、製品の純度は、99.5％であった。The supply of the raw material liquid was stopped when the amount of the raw material liquid in the crystallization chamber (25) was filled, and then pressure crystallization separation was performed.
This pressure crystallization separation is performed by lowering the piston (19) to 1500
After pressurizing to Kg / cm 2 to further increase the slurry concentration, the piston (19) is further lowered to remove the liquid phase component from the filter (21),
Separation and discharge were performed through the discharge pipe line (20), and subsequently, while adjusting the pressure applied to the liquid phase, the liquid phase components generated by the reduced pressure perspiration phenomenon were separated and compressed. This depressurized sweating operation was continued until the pressure applied to the liquid phase reached a substantially constant value near atmospheric pressure. The maximum differential pressure for pressing was 600 Kg / cm 2 . Results of such pressure crystallization separation of nuclear, P- cresol aimed product was obtained 649 g r. The yield is 43.3%
And was much higher than the yield in Comparative Example 1 below. The product purity was 99.5%.
比較例１ 比較例１（従来法）に使用した圧力晶析分離設備は、
予冷槽と、ポンプと、圧力晶析分離装置とが、この順に
管接続されたものである。上記予冷槽、ポンプ及び圧力
晶析分離装置の構成、能力等、また、圧力晶析分離用の
原料液及び目的製品等は、全て実施例１と同様である。Comparative Example 1 The pressure crystallization separation equipment used in Comparative Example 1 (conventional method) is
A precooling tank, a pump, and a pressure crystallization separator are connected in this order by pipes. The configurations and capacities of the precooling tank, the pump, and the pressure crystallization separator, the raw material liquid for pressure crystallization separation, the target product, and the like are all the same as in Example 1.
原料液を予冷槽にて15℃に予冷却した。予冷却後のス
ラリ濃度は18.3％であった。予冷却後、配管のバルブを
開き、ポンプを作動させ、予冷却された原料液を3.0/
minの流速で圧力晶析分離装置へ供給した。晶析室に到
達したときの原料液の温度は17.0℃であり、予冷後の温
度より高くなった。晶析室に原料液が満たされた時点で
原料液の供給を停止し、ついで圧力晶析分離を行った。
この圧力晶析分離は、実施例１と同様の操作方法により
行った。圧力晶析分離の結果、目的製品とするＰ−クレ
ゾールが529gr得られた。その収率は35.3％である。
尚、製品の純度は99.5％であった。The raw material liquid was precooled to 15 ° C in a precooling tank. The slurry concentration after precooling was 18.3%. After precooling, open the piping valve and operate the pump to remove the precooled raw material liquid to 3.0 /
It was supplied to the pressure crystallization separator at a flow rate of min. The temperature of the raw material liquid when it reached the crystallization chamber was 17.0 ° C, which was higher than the temperature after precooling. When the crystallization chamber was filled with the raw material liquid, the supply of the raw material liquid was stopped, and then pressure crystallization separation was performed.
This pressure crystallization separation was performed by the same operation method as in Example 1. Result of the pressure crystallization separation, P- cresol aimed product was obtained 529 g r. Its yield is 35.3%.
The product purity was 99.5%.
（発明の効果） 本発明の圧力晶析分離設備および圧力晶析分離方法
は、予冷槽での原料液の過冷却をすることなく、又、元
の原料液中の成分濃度を低めることなく、予冷槽により
予冷却されて圧力晶析分離に必要な所定温度（T0）に調
整された原料液（スラリ液）を、熱交換器への冷却用熱
媒の循環により予冷却後熱量除去しながら圧力晶析分離
装置へ供給することができ、それにより、予冷槽により
予冷却されて圧力晶析分離に必要な所定温度（T0）に調
整された原料液（スラリ液）が圧力晶析分離装置の晶析
室へ供給され、到達した時の原料液の温度を圧力晶析分
離に必要な温度（T0）にでき、そして圧力晶析分離を行
うことができる。(Effect of the invention) The pressure crystallization separation equipment and the pressure crystallization separation method of the present invention, without supercooling the raw material liquid in the precooling tank, and without lowering the component concentration in the original raw material liquid, The raw material liquid (slurry liquid) that has been pre-cooled by the pre-cooling tank and adjusted to the predetermined temperature (T 0 ) required for pressure crystallization separation is pre-cooled to remove heat by circulating the cooling heat medium to the heat exchanger. However, the raw material liquid (slurry liquid) pre-cooled by the pre-cooling tank and adjusted to the predetermined temperature (T 0 ) necessary for pressure crystallization separation can be supplied to the pressure crystallization separation device. The temperature of the raw material liquid when it is supplied to the crystallization chamber of the separation device and reaches it can be adjusted to the temperature (T 0 ) required for pressure crystallization separation, and pressure crystallization separation can be performed.
又、熱交換器に循環する熱媒を冷却用熱媒から保温用
熱媒に直ちに切り換えることができることから、原料液
送給後から次の原料液送給開始前にいたる原料液送給停
止の間、熱交換器に保温用熱媒を循環することができ、
それにより、原料液送給停止の間における原料液送給管
内の原料液の温度低下による固化や原料液の固化による
原料液送給管の閉塞を防止でき、その結果、以降の運転
の継続の困難化や不能化等の支障を生じることなく、次
の原料液送給を円滑に行うことができる。In addition, since the heat medium circulating in the heat exchanger can be immediately switched from the cooling heat medium to the heat retaining heat medium, the feed of the raw material liquid is stopped after the feed of the raw material liquid and before the start of the next feed of the raw material liquid. During that time, a heat carrier for heat insulation can be circulated in the heat exchanger,
As a result, it is possible to prevent the solidification of the raw material liquid in the raw material liquid supply pipe due to the temperature drop during the raw material liquid supply stoppage and the blockage of the raw material liquid supply pipe due to the solidification of the raw material liquid. It is possible to smoothly feed the next raw material liquid without causing troubles such as difficulty and disabling.
従って、本発明によれば、予冷操作の困難化、予冷槽
の能力増強、原料液の送給不可、運転の継続の困難化及
び不能化などを招くことなく、目的製品収率の向上が図
れる。Therefore, according to the present invention, the target product yield can be improved without making the precooling operation difficult, the capacity enhancement of the precooling tank, the inability to feed the raw material liquid, the difficulty and the discontinuity of the operation, and the like. .
第１図は、本発明の実施例に係るプロセスフローを示す
図、第２図は、圧力晶析分離装置の概念を示す図、第３
図は、従来のプロセスフローを示す図である。 （１）……圧力容器、（２）……下蓋、（３）……油圧
ユニット、（４）……晶析室、 （５）……ピストン、（６）……排液タンク、（７）…
…予備晶析缶、 （８）……原料供給ポンプ、（９）（13）……配管、
（10）……減圧機構、 （11）（12）（16）……弁、（14）……原料タンク、
（15）……オーバーフロー管、 （17）……高圧容器の胴部、（18）……高圧容器の下蓋
部、（19）……ピストン、 （20）……排出管路、（21）……フィルタ、（22）……
原料液供給用配管、 （23）……断熱板、（24）……ヒータ、（25）……晶析
室、 （26）……断熱支持材、（27）……予冷槽、（28）……
ポンプ、 （29）……熱交換器、（30）……冷却用熱媒槽、（31）
……保温用熱媒槽、 （32）……圧力晶析分離装置、A1,A2,A3……温度測定
器。FIG. 1 is a diagram showing a process flow according to an embodiment of the present invention, FIG. 2 is a diagram showing a concept of a pressure crystallization separator, and FIG.
The figure shows a conventional process flow. (1) ... pressure vessel, (2) ... lower lid, (3) ... hydraulic unit, (4) ... crystallization chamber, (5) ... piston, (6) ... drainage tank, ( 7) ...
… Preliminary crystallization can, (8) …… Raw material supply pump, (9) (13) …… Piping,
(10) …… Decompression mechanism, (11) (12) (16) …… Valve, (14) …… Material tank,
(15) …… Overflow pipe, (17) …… Body of high pressure container, (18) …… Lower lid of high pressure container, (19) …… Piston, (20) …… Discharge pipe, (21) …… Filter, (22) ……
Raw material liquid supply pipe, (23) …… insulating plate, (24) …… heater, (25) …… crystallization chamber, (26) …… insulating support material, (27) …… precooling tank, (28) ......
Pump, (29) …… Heat exchanger, (30) …… Heat medium tank for cooling, (31)
...... Heat carrier for heat insulation, (32) …… Pressure crystallization separator, A 1 , A 2 , A 3 …… Temperature measuring instrument.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｂ０１Ｄ 9/02 ６２１ 9344−4Ｄ ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification code Internal reference number FI technical display location B01D 9/02 621 9344-4D
Claims (2)
を予冷槽から圧力晶析分離装置へ送給するポンプと、送
給された原料液の圧力晶析分離を行う圧力晶析分離装置
とを有する圧力晶析分離設備において、前記ポンプと前
記圧力晶析分離装置との間に、冷却用熱媒槽及び保温用
熱媒槽を付帯した熱交換器を接続してなることを特徴と
する圧力晶析分離設備。1. A precooling tank for a raw material liquid for pressure crystallization separation, a pump for feeding the raw material liquid from the precooling tank to a pressure crystallization separator, and a pressure crystal for performing pressure crystallization separation of the fed raw material liquid. In a pressure crystallization separation facility having a crystallization separator, a heat exchanger having a cooling heat medium tank and a heat retaining heat medium tank is connected between the pump and the pressure crystallization separator. Pressure crystallization separation equipment characterized by.
原料液を原料液送給用ポンプで圧力晶析分離装置へ供給
し、圧力晶析分離することを繰り返して行う圧力晶析分
離方法において、前記圧力晶析分離装置への原料液供給
の間、前記予冷却された原料液から、原料液が圧力晶析
分離装置の高圧容器壁内に位置する原料液供給用配管内
を通過する際に高圧容器壁から受ける入熱量に相当する
熱量を、原料液送給用ポンプと圧力晶析分離装置との間
で、この間に接続した熱交換器に冷却用熱媒を導入する
ことにより除去しながら、圧力晶析分離装置への原料液
供給を行い、この原料液供給後から次の原料液供給開始
前にいたる原料液供給停止の間、上記熱交換器に保温用
熱媒を導入することを特徴とする圧力晶析分離方法。2. A pressure crystallization in which a raw material liquid precooled to a temperature required for pressure crystallization separation is supplied to a pressure crystallization separator by a raw material liquid feed pump and pressure crystallization is repeated. In the separation method, during the supply of the raw material liquid to the pressure crystallization separation device, from the pre-cooled raw material liquid, the raw material liquid inside the high pressure vessel wall of the pressure crystallization separation device in the raw material liquid supply pipe Introduce a heat quantity corresponding to the heat quantity received from the wall of the high-pressure vessel when passing between the raw material liquid feed pump and the pressure crystallization separator into the heat exchanger for cooling, which is connected to the heat exchanger. While supplying the raw material liquid to the pressure crystallization separator while removing it, during the supply of the raw material liquid after the supply of the raw material liquid and before the start of the next raw material liquid supply, the heat-transfer heat medium is supplied to the heat exchanger. A pressure crystallization separation method characterized by introducing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63035824A JPH082402B2 (en) | 1988-02-18 | 1988-02-18 | Pressure crystallization separation equipment and pressure crystallization separation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63035824A JPH082402B2 (en) | 1988-02-18 | 1988-02-18 | Pressure crystallization separation equipment and pressure crystallization separation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01210001A JPH01210001A (en) | 1989-08-23 |
| JPH082402B2 true JPH082402B2 (en) | 1996-01-17 |
Family
ID=12452703
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63035824A Expired - Fee Related JPH082402B2 (en) | 1988-02-18 | 1988-02-18 | Pressure crystallization separation equipment and pressure crystallization separation method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH082402B2 (en) |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS62176503A (en) * | 1986-01-30 | 1987-08-03 | Kobe Steel Ltd | Pressure crystallization control method and device therefor |
-
1988
- 1988-02-18 JP JP63035824A patent/JPH082402B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01210001A (en) | 1989-08-23 |
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