JPH026801A - Pressure crystallization method - Google Patents
Pressure crystallization methodInfo
- Publication number
- JPH026801A JPH026801A JP15869488A JP15869488A JPH026801A JP H026801 A JPH026801 A JP H026801A JP 15869488 A JP15869488 A JP 15869488A JP 15869488 A JP15869488 A JP 15869488A JP H026801 A JPH026801 A JP H026801A
- Authority
- JP
- Japan
- Prior art keywords
- pressure
- reached
- predetermined
- crystallization
- amount
- 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.)
- Granted
Links
- 238000002425 crystallisation Methods 0.000 title claims abstract description 61
- 239000013078 crystal Substances 0.000 claims abstract description 48
- 238000000926 separation method Methods 0.000 claims abstract description 25
- 239000002002 slurry Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 31
- 239000002994 raw material Substances 0.000 claims description 25
- 238000006073 displacement reaction Methods 0.000 claims description 20
- 230000015572 biosynthetic process Effects 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 16
- 239000000126 substance Substances 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 2
- 230000008025 crystallization Effects 0.000 abstract description 33
- 239000000463 material Substances 0.000 abstract description 25
- 239000007787 solid Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 23
- 230000007423 decrease Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000008569 process Effects 0.000 description 4
- 238000007711 solidification Methods 0.000 description 4
- 230000008023 solidification Effects 0.000 description 4
- 239000012265 solid product Substances 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000011038 discontinuous diafiltration by volume reduction Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000010926 purge Methods 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
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、圧力晶析方法に関し、詳細には、特に結晶成
長速度の小さい物質系の圧力晶析方法に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a pressure crystallization method, and more particularly to a pressure crystallization method for a material system with a low crystal growth rate.
（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
な原料系への通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、高収率が得易い事、及び、エネル
ギ消費量が少ない事等から、近年の化学工業のファイン
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
。(Conventional technology) The pressure crystallization method has great potential for application to raw materials that are difficult to separate using conventional distillation methods and cooling crystallization methods, it is easy to obtain high-purity products, and Due to its easy yield and low energy consumption, it is a separation and purification technology that has been attracting a lot of attention as the chemical industry has become increasingly refined in recent years.
かかる圧力晶析法の概要は、例えば、化学工業５０巻（
１９８６年）３３１頁「圧力晶析法と装置の概要」に記
載されている。これを第１図（プロセスフロー及び装置
の概念を示す図）によって説明すると、圧力容器（１）
には、下方に蓋体（下！り（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
にて上下動するように設けられており、このピストン（
５）と下蓋（２）とによって圧力容ｉ？ｆ）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）とは、減圧機構Ｇ■及び弁０１）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）とは、原料供給ポンプ（８）、弁０２）を介し
て配管側により連結されている。An overview of this pressure crystallization method can be found, for example, in Kagaku Kogyo Volume 50 (
(1986), p. 331, "Outline of pressure crystallization method and apparatus". To explain this using Figure 1 (a diagram showing the process flow and the concept of the device), the pressure vessel (1)
is provided with a lid (2) at the bottom, and a piston (5) is provided to move up and down within the container (1) by the operation of a hydraulic unit (3). (
5) and the lower cover (2), the pressure capacity i? f) A crystallization chamber (4) is formed within the crystallization chamber (4). This crystallization chamber (4) and the drain tank (
6) means the pipe (9) via the pressure reducing mechanism G■ and valve 01).
) are connected. Further, the crystallization chamber (4) and the pre-crystallizer (7) are connected to each other by a piping side via a raw material supply pump (8) and a valve 02).
この装置において、原料は原料タンク０滲より予備晶析
缶（７）に送給され、ここで冷却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 apparatus, the raw material is fed from the raw material tank 0 to the pre-crystallizer (7), where it is cooled to produce seed crystals for pressure crystallization. This is because when raw materials without seed crystals are subjected to pressure crystallization, the supersaturation pressure is generally relatively high, typically several hundred atmospheres or more, and high pressure is required for initial crystal formation. This is because there is a risk that the slurry containing seed crystals will be supplied, which has the advantage that not only is there no need to worry about such supersaturation pressure, but crystal growth can be expected without nucleation due to pressurization.
次に、配管０りから弁０２１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θつを通
って液流出が始まるので、これを検知して弁０２）、０
ω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、断熱的に加圧する
方法が採用される。Next, the raw material is transferred from the pipe 0 to the crystallization chamber (4) via the valve 021.
). When the crystallization chamber (4) is filled with the raw material, the liquid begins to flow out through two overflow pipes θ having openings at the tip of the piston.This is detected and the valves 02) and 0
ω is closed and pressurization by the piston (5) is started. When the raw material liquid is pressurized, crystallization of specific substances in the raw material progresses,
The inside of the crystallization chamber (4) is in a solid-liquid equilibrium state under high pressure. The solid produced at this time is generally a substance of extremely high purity. Note that the temperature inside the crystallization chamber (4) rises due to the latent heat of solidification generated as solidification progresses, but in the pressure crystallization method, cooling is generally not performed to prevent this temperature rise, and heating is performed adiabatically. A pressure method is adopted.
次に、所定の圧力まで昇圧すると、−船釣には直ちに晶
析が完了し、所定の固液比率（飽和状態）に達するので
、この圧力を検知すると直ちに弁（１１）を開き、固液
分離を開始する。そして、弁（１１）開の状態で、油圧
ユニット（３）からピストン（５）に作用する圧力を保
持したままピストンの下降を続けると、晶析室（４）内
の圧力は一定に保持された状態で液相が晶析室（４）か
ら排液タンク（６）に排出される。Next, when the pressure is increased to a predetermined pressure, crystallization is immediately completed and the predetermined solid-liquid ratio (saturation state) is reached. When this pressure is detected, the valve (11) is immediately opened and the solid-liquid ratio is reached. Begin separation. Then, with the valve (11) open, if the piston continues to descend while maintaining the pressure acting on the piston (5) from the hydraulic unit (3), the pressure in the crystallization chamber (4) will be maintained constant. The liquid phase is discharged from the crystallization chamber (4) into the drain tank (6) in the same state.
更にピストン（５）の下降を継続すると晶析室（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。Further, as the piston (5) continues to descend, the crystal grains in the crystallization chamber (4) are compressed and the remaining liquid between the crystal grains is discharged into the drain tank (6) through the so-called "squeezing action". be done.
ピストン（５）の下降が更に続（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。この様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。As the piston (5) continues to descend, the crystal grains are formed into one large lumpy solid product along the shape of the crystallization chamber (4). At the stage of separation, the liquid phase pressure in the crystallization chamber (4), which is connected to the drain tank (6) under atmospheric pressure, gradually decreases, so the crystal surface partially melts. A so-called "sweating wash" is carried out to purify the bulk solid product.
晶析室（４）から排出される排液の圧力が所定の圧力に
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Ｑ５１内の残液を、窒素ガ
ス等の製品に対して不活性なガスでパージし、次工程の
注入時の満液検知の為の４！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 piston (5) stops descending, and at the same time the piston begins to rise, the high pressure container (1) also rises. , the solid product is removed from the container (1) while being placed on the lower lid (2). This is the product removal device (
(not shown), lower the high-pressure container (1) and attach it to the lower lid (2), and then return to the raw material injection process.
The same process will be repeated.Before injecting the raw material, purge the remaining liquid in the overflow pipe Q51 with a gas inert to the product, such as nitrogen gas, and then 4 for full liquid detection! Be prepared.
以上の工程を繰り返すことによって製品を連続的に生産
する。By repeating the above steps, products are produced continuously.
（発明が解決しようとする課題）
ところが、従来の圧力晶析方法は、所期の製品収率に比
較し、実際得られる製品収率が低い場合がある。この収
率の改善を図るべく、種々検討したところ、この収率低
下は結晶成長速度の小さい物質系において特に顕著であ
ることが判った。そして、結晶成長速度が小さい程、収
率低下が大きい事が確認された。このように従来の圧力
晶析方法は、結晶成長速度の小さい物質系において製品
収率が低いという問題点がある。(Problems to be Solved by the Invention) However, in the conventional pressure crystallization method, the actually obtained product yield may be lower than the expected product yield. As a result of various studies aimed at improving this yield, it was found that this decrease in yield is particularly remarkable in material systems with low crystal growth rates. It was also confirmed that the lower the crystal growth rate, the greater the decrease in yield. As described above, the conventional pressure crystallization method has a problem in that the product yield is low in material systems with a low crystal growth rate.
本発明は、この様を事情に着目してなされたものであっ
て、その目的は結晶成長速度の小さい物質系（原料）を
圧力晶析するに当たり、その製品収率の改善を図り得る
圧力晶析方法を提供しようとするものである。The present invention was made in view of these circumstances, and its purpose is to provide a pressure crystallizer that can improve the product yield when pressure crystallizing a material system (raw material) with a low crystal growth rate. The purpose of this study is to provide an analysis method.
（課題を解決するための手段）
上記課題を達成するために、本発明は次のような構成の
圧力晶析方法としている。即ち、第１請求項の方法は、
高圧容器内に液状又はスラリ状原料を供給し、該容器内
にて該原料を所定圧まで加圧して晶析した後、加圧下で
液相分を該容器外に排出して固液分離し、晶析物質を得
る圧力晶析方法において、前記所定圧に到達した後該圧
力に保持し、該圧力保持状態で結晶生成量が所定量に達
したことを検知してから、前記固液分離を開始すること
を特徴とする圧力晶析方法である。第２請求項の方法は
、高圧容器内温度が予め設定された値に到達した事を検
知する事により、前記結晶生成量の所定量到達の検知を
行う第１請求項に記載の圧力晶析方法である。第３請求
項の方法は、高圧容器内への供給原料の温度と加圧後の
高圧容器内温度との差を検出して昇温■を求め、該昇温
量が予め設定された値に到達した事を検知する事により
、前記結晶生成量の所定量到達の検知を行う第１請求項
に記載の圧力晶析方法である。第４請求項の方法は、加
圧用ピストンを有する高圧容器を用い、加圧後のピスト
ンの変移を検出し、該変移が予め設定された値に到達し
た事を検知する事により、前記結晶生成量の所定量到達
の検知を行う第１請求項に記載の圧力晶析方法である。(Means for Solving the Problems) In order to achieve the above problems, the present invention provides a pressure crystallization method having the following configuration. That is, the method of the first claim:
A liquid or slurry raw material is supplied into a high-pressure container, and after the raw material is pressurized to a predetermined pressure in the container to crystallize, the liquid phase is discharged outside the container under pressure to perform solid-liquid separation. In the pressure crystallization method for obtaining a crystallized substance, after reaching the predetermined pressure, the pressure is maintained, and after detecting that the amount of crystal formation has reached the predetermined amount while the pressure is maintained, the solid-liquid separation is performed. This is a pressure crystallization method characterized by starting. The method according to the second claim is the pressure crystallization method according to the first claim, which detects that the amount of crystal formation has reached a predetermined amount by detecting that the temperature inside the high-pressure container has reached a preset value. It's a method. The method according to the third aspect detects the difference between the temperature of the raw material to be fed into the high-pressure container and the temperature inside the high-pressure container after pressurization to determine the temperature increase (■), and the temperature increase amount is adjusted to a preset value. The pressure crystallization method according to claim 1, wherein the arrival of the predetermined amount of crystal production is detected by detecting that the amount of crystal production has reached the predetermined amount. The method of claim 4 uses a high-pressure container having a pressurizing piston, detects the displacement of the piston after pressurization, and detects that the displacement reaches a preset value, thereby generating the crystals. The pressure crystallization method according to claim 1, wherein reaching a predetermined amount is detected.
第５請求項の方法は、前記所定圧に到達した後のピスト
ンの変移が予め設定された値に到達した事を検知する事
により、前記結晶生成量の所定量到達の検知を行う第４
請求項に記載の圧力晶析方法である。また、第６請求項
の方法は、前記所定圧に到達した後、予め設定された一
定時間該圧力に保持し、次いで前記固液分離を開始する
ことを特徴とする請求
方法である。The method according to claim 5 includes a method for detecting that the amount of crystal formation has reached a predetermined amount by detecting that the displacement of the piston after reaching the predetermined pressure has reached a preset value.
A pressure crystallization method according to the claims. The method according to claim 6 is characterized in that after reaching the predetermined pressure, the pressure is maintained for a predetermined period of time, and then the solid-liquid separation is started.
（作用および実施例）
結晶成長速度の小さい物質系において製品収率が低い原
因に関して検討した結果に基づき、以下説明する。(Operations and Examples) Based on the results of an investigation into the causes of low product yields in material systems with low crystal growth rates, explanations will be given below.
第２図に、加圧後における時間（横軸：Ｌ）と高圧容器
内圧力及び温度（縦軸：Ｐ，？）との関係を示す。この
例は、所定圧力ｒｅに達するまで加圧した後、該圧力Ｐ
ｅに保持し続けたときのものである。FIG. 2 shows the relationship between the time after pressurization (horizontal axis: L) and the internal pressure and temperature of the high-pressure container (vertical axis: P, ?). In this example, after pressurizing until a predetermined pressure re is reached, the pressure P
This is what happens when it continues to be held at e.
図中Ｐは圧力、Ｔａは結晶成長速度の大きい物質系Ａの
場合の温度、Ｔｂは結晶成長速度の小さい物質系Ｂの場
合の温度を示している。In the figure, P indicates the pressure, Ta indicates the temperature in the case of material system A with a high crystal growth rate, and Tb indicates the temperature in the case of material system B with a low crystal growth rate.
この図から判る様に、圧力Ｐが１，秒後に所定圧力Ｐｅ
に達すると、物質系Ａの場合はほぼ同時に昇温が終了し
、温度Ｔａが最高温度Ｔｅに達している。As can be seen from this figure, the pressure P changes to the predetermined pressure Pe after 1 second.
When the temperature Ta reaches the maximum temperature Te, the temperature increase for the material system A ends almost at the same time.
ところが、物質系Ｂの場合は、所定圧力Ｐｅに達しても
昇温のｉ８渡朋にあり、ｔ２秒後に最高温度Ｔｅに達す
る。However, in the case of material system B, even when the predetermined pressure Pe is reached, the temperature is still rising at i8, and reaches the maximum temperature Te after t2 seconds.
この昇温は、晶析の進行に伴って発生する固化潜熱によ
るものである。故に、物質系Ｂの場合は、所定圧力Ｐｅ
に達しても、未だ晶析が進行中である。従って、所定圧
力Ｐｅ到達後、すぐに固液分離を開始すると晶析が未完
了の状態で固液分離されてしまうため製品収率が低くな
る。これが、従来の圧力晶析方法において結晶成長速度
の小さい物質系の場合に製品収率が低くなる原因である
。This temperature increase is due to latent heat of solidification generated as crystallization progresses. Therefore, in the case of material system B, the predetermined pressure Pe
Even after reaching , crystallization is still in progress. Therefore, if solid-liquid separation is started immediately after the predetermined pressure Pe is reached, solid-liquid separation will occur before crystallization is completed, resulting in a low product yield. This is the reason why product yields are low in conventional pressure crystallization methods for material systems with low crystal growth rates.
即ち、従来の方法は、所定圧に到達すると直ちに弁（１
１）を開き、液相分を該容器外に排出して固液分離を開
始するものである。故に、結晶成長速度の大きい物質系
の場合は、所定圧に達すると直ちに晶析が完了するので
、所定圧到達後すぐに固液分離が開始されても所期の製
品収率が得られる。That is, in the conventional method, as soon as the predetermined pressure is reached, the valve (1
1) is opened, the liquid phase is discharged out of the container, and solid-liquid separation is started. Therefore, in the case of a substance system with a high crystal growth rate, crystallization is completed as soon as the predetermined pressure is reached, so even if solid-liquid separation is started immediately after the predetermined pressure is reached, the desired product yield can be obtained.
しかし、結晶成長速度の小さい′＋！ｆＪｉ系の場合は
所定圧に達しても未だ晶析が完了していないので、晶析
未完了の状態で固液分離されてしまう。そのために製品
収率が低いものとなるのである。However, the crystal growth rate is low ′+! In the case of the fJi system, crystallization is not yet completed even when the predetermined pressure is reached, so solid-liquid separation occurs in an incomplete state of crystallization. This results in a low product yield.
この製品収率を改善するには、所定圧力Ｐｅに保持した
状態で結晶生成量が所定量に達してから固液分離を開始
するようにすればよい。このとき最高温度Ｔｅに達する
１２秒後に、固液分離を開始すると、最高の製品収率が
得られる。In order to improve this product yield, solid-liquid separation may be started after the amount of crystal formation reaches a predetermined amount while maintaining the pressure at a predetermined pressure Pe. At this time, if solid-liquid separation is started 12 seconds after reaching the maximum temperature Te, the highest product yield can be obtained.
そこで、本発明に係る圧力晶析方法は、前に説明したよ
うに、高圧容器内にて原料を所定圧に到達した後該圧力
に保持し、該圧力保持状態で結晶生成量が所定量に達し
たことを検知してから、前記固液分離を開始するように
している。このようにすると、結晶成長速度の小さい物
質系の場合でも、製品収率を高いものにし得るのである
。Therefore, as explained above, in the pressure crystallization method according to the present invention, after the raw material reaches a predetermined pressure in a high-pressure container, it is maintained at that pressure, and while the pressure is maintained, the amount of crystal formation reaches a predetermined amount. After detecting that the solid-liquid separation has been reached, the solid-liquid separation is started. In this way, even in the case of a material system with a low crystal growth rate, a high product yield can be achieved.
上記結晶生成量が所定量に到達した事（以降、所定量到
達という）を検知する具体的方法に関して、以下に述べ
る。A specific method for detecting that the amount of crystal formation has reached a predetermined amount (hereinafter referred to as reaching the predetermined amount) will be described below.
前記の如く、昇温は晶析の進行に伴って発生する固化潜
熱によるものであるので、温度と結晶生成量とは密接な
関係がある。従って、予めこの関係を求め、それに基づ
き所定の結晶生成量に対応する温度を設定しておき、該
設定値に到達した事を検知すれば、所定量到達を検知で
きる。As mentioned above, since the temperature increase is due to the latent heat of solidification generated as crystallization progresses, there is a close relationship between the temperature and the amount of crystal formation. Therefore, by determining this relationship in advance, setting the temperature corresponding to a predetermined amount of crystal formation based on it, and detecting that the set value has been reached, it is possible to detect that the predetermined amount has been reached.
ところで、温度と結晶生成量との関係は、晶析開始温度
、即ち・原料供給温度によって異なる。この温度は、種
々の要因により、時として１°Ｃ程度の変動はあり得る
と考えるべきである。従って、高圧容器内への供給原料
の温度と加圧後の高圧容器内温度との差を検出して昇温
量を求め、該昇温量が予め設定された値に到達した事を
検知する事により、所定量到達の検知を行う方がより望
ましい。尚、この昇温量は、第２図ではΔＴで示される
ものである。Incidentally, the relationship between temperature and the amount of crystal formation varies depending on the crystallization start temperature, that is, the raw material supply temperature. It should be considered that this temperature may sometimes fluctuate by about 1°C due to various factors. Therefore, the amount of temperature increase is determined by detecting the difference between the temperature of the raw material fed into the high-pressure container and the temperature inside the high-pressure container after pressurization, and it is detected that the amount of temperature increase has reached a preset value. In some cases, it is more desirable to detect when a predetermined amount has been reached. Note that this temperature increase amount is indicated by ΔT in FIG.
また、前記の如く、最高の製品収率を得るためには、最
高温度Ｔｅに達してから固液分離を開始すればよいが、
最高温度Ｔｅに達する迄に長時間を要する様な場合には
、！サイクル（原料供給から製品取り出しまで）に要す
る時間が長くなり、単位時間当たりの生産量が低下する
。従って、この様な場合は、製品収率と生産量とのバラ
ンスを考慮し、ある程度の温度或いは昇温量に達した時
点、例えば時間１，１秒後の時点で固液分離を開始する
のが好ましい。Furthermore, as mentioned above, in order to obtain the highest product yield, solid-liquid separation should be started after reaching the maximum temperature Te;
If it takes a long time to reach the maximum temperature Te,! The time required for the cycle (from raw material supply to product removal) becomes longer, and the production volume per unit time decreases. Therefore, in such cases, considering the balance between product yield and production amount, it is recommended to start solid-liquid separation when a certain temperature or amount of temperature increase is reached, for example, after 1.1 seconds. is preferred.
第３図に、加圧後における時間（横軸：ｔ）と高圧容器
内圧力及びピストンの変移（縦軸：Ｐ、Ｌ）との関係を
示す。図中Ｐは圧力、Ｌａは結晶成長速度の大きい物質
系への場合のピストン変移、Ｌｂは結晶成長速度の小さ
い物質系Ｂの場合のピストン変移を示している。FIG. 3 shows the relationship between the time after pressurization (horizontal axis: t), the pressure inside the high-pressure container, and the displacement of the piston (vertical axis: P, L). In the figure, P indicates pressure, La indicates piston displacement in the case of a material system with a high crystal growth rate, and Lb indicates piston displacement in the case of material system B with a low crystal growth rate.
この図から判る様に、圧力Ｐが１１秒後に所定圧力Ｐｅ
に達すると、物質系Ａの場合のピストン変移Ｌａはほぼ
同時に一定値Ｌｅ（最高値）に到達する。As can be seen from this figure, the pressure P changes to the predetermined pressure Pe after 11 seconds.
, the piston displacement La for material system A reaches a constant value Le (maximum value) almost at the same time.
ところが、物質系Ｂの場合は、所定圧力Ｐｅに達しても
ピストン変移の過渡期にあり、１２秒後に一定値Ｌｅに
達する。However, in the case of material system B, even when the predetermined pressure Pe is reached, the piston is still in the transition period of displacement, and reaches the constant value Le after 12 seconds.
このピストン変移は、晶析に伴う体積減少によるもので
ある。故に、物質系Ｂの場合は、所定圧力Ｐｅに達して
も、未だ晶析が進行中である。This piston displacement is due to volume reduction accompanying crystallization. Therefore, in the case of material system B, even if the predetermined pressure Pe is reached, crystallization is still in progress.
上記のようにピストン変移と結晶生成量とは密接な関係
がある。従って、予めこの関係を求め、それに基づき所
定の結晶生成層に対応するピストン変移を設定しておき
、該設定値に到達した事を検知すれば、所定量到達を検
知できる。As mentioned above, there is a close relationship between the piston displacement and the amount of crystal formation. Therefore, by determining this relationship in advance, setting the piston displacement corresponding to a predetermined crystal formation layer based on it, and detecting that the set value has been reached, it is possible to detect that the predetermined amount has been reached.
ところで、ピストン変移と結晶生成量との関係は、晶析
開始時点のピストン位置によって異なる。このピストン
位置は、種々の要因により異なり、多少の変動はあり得
ると考えるべきである。従って、所定圧に到達した後の
ピストンの変移が予め設定された値に到達した事を検知
する事により、所定量到達の検知を行う方が望ましい。Incidentally, the relationship between the piston displacement and the amount of crystal formation differs depending on the piston position at the time of starting crystallization. This piston position varies depending on various factors and should be considered to be subject to some variation. Therefore, it is preferable to detect that the predetermined amount has been reached by detecting that the displacement of the piston after reaching the predetermined pressure has reached a preset value.
尚、この変移は、第３図ではΔして示すものである。Note that this transition is indicated by Δ in FIG.
また、最高の製品収率を得るためには、ピストン変移が
一定値Ｌｅ、或いはＬｅに相当するΔＬに到達してから
固液分離を開始すればよいが、これらの値に達する迄に
長時間を要する様な場合には、単位時間当たりの生産量
が低下する。従って、この様な場合は、製品収率と生産
量とのバランスを考慮し、ある程度のピストン変移に達
した時点、例えば変位Ｌｆに到達した時点で固液分離を
開始するのが好ましい。In addition, in order to obtain the highest product yield, solid-liquid separation should be started after the piston displacement reaches a constant value Le or ΔL corresponding to Le, but it takes a long time to reach these values. If this is required, the production amount per unit time will decrease. Therefore, in such a case, considering the balance between product yield and production amount, it is preferable to start solid-liquid separation when the piston reaches a certain level of displacement, for example, when the displacement Lf is reached.
また、第２図、第３図から明らかなように、第２図及び
第３図の共通座標軸である時間（Ｄを管理し、時間が＋
２又はり、に達した事を検出して固液分離を開始するこ
とも可能である。In addition, as is clear from Figs. 2 and 3, time (D, which is a common coordinate axis in Figs. 2 and 3) is managed, and time +
It is also possible to start solid-liquid separation by detecting that 2 or more has been reached.
（発明の効果）
本発明に係る圧力晶析方法によれば、結晶成長速度の小
さい物質系（原料）を圧力晶析する際、製品収率が改善
され、所期の高い製品収率が得られるようになる。(Effects of the Invention) According to the pressure crystallization method according to the present invention, when pressure crystallizing a material system (raw material) with a low crystal growth rate, the product yield is improved and the desired high product yield can be obtained. You will be able to do it.
第１図は、圧力晶析方法に係るプロセスフロー及び装置
の概念を示す閏、第２図は、加圧後における時間（横軸
；ｔ）と高圧容器内圧力及び温度（縦軸：Ｐ、Ｔ）との
関係を示す図、第３図は、加圧後における時間（横軸：
ｔ）と高圧容器内圧力及びピストンの変移（紺軸：Ｐ、
Ｌ）との関係を示す図である。
（１）−一〜−圧力容器 （２）−−−一下蓋（３
）−−−一油圧ユニット （４Ｌ−一一晶析室（５）−
−−−ピストン （６）−−−一排液タンク（７）
−−−一子備晶折缶 （８）−−−一原料供給ポンプ
（９）０り一一一一配管 ＧＯ）−−−一濾圧機
構（Ｉｌｌ（１２）（１６）
原料タンク
（＋５）−、オーバーフロー管
特許出願人 株式会社 神戸製鋼所
代 理 人 弁理士 全光 章−Figure 1 shows the process flow and the concept of the device related to the pressure crystallization method. Figure 2 shows the time after pressurization (horizontal axis; t) and the pressure and temperature inside the high-pressure vessel (vertical axis: P, Figure 3 shows the relationship between T) and time after pressurization (horizontal axis:
t) and the pressure inside the high-pressure container and the displacement of the piston (dark blue axis: P,
It is a figure showing the relationship with L). (1) -1~-Pressure vessel (2)---1 lower lid (3
)---1 Hydraulic unit (4L-11 Crystallization chamber (5)-
--- Piston (6) --- Drainage tank (7)
---Ichikobisho folding can (8) ---1 Raw material supply pump (9) 01111 piping GO) ---1 Filtration pressure mechanism (Ill (12) (16) Raw material tank (+5) )−, overflow pipe patent applicant Kobe Steel Co., Ltd. agent Patent attorney Akira Zenko−
Claims (6)
容器内にて該原料を所定圧まで加圧して晶析した後、加
圧下で液相分を該容器外に排出して固液分離し、晶析物
質を得る圧力晶析方法において、前記所定圧に到達した
後該圧力に保持し、該圧力保持状態で結晶生成量が所定
量に達したことを検知してから、前記固液分離を開始す
ることを特徴とする圧力晶析方法。(1) Supply a liquid or slurry raw material into a high-pressure container, pressurize the raw material to a predetermined pressure in the container to crystallize it, and then discharge the liquid phase out of the container under pressure to solidify it. In a pressure crystallization method for obtaining a crystallized substance by liquid separation, after reaching the predetermined pressure, the pressure is maintained, and after detecting that the amount of crystal formation has reached the predetermined amount while the pressure is maintained, A pressure crystallization method characterized by starting solid-liquid separation.
を検知する事により、前記結晶生成量の所定量到達の検
知を行う第１請求項に記載の圧力晶析方法。(2) The pressure crystallization method according to claim 1, wherein reaching a predetermined amount of crystal formation is detected by detecting that the temperature inside the high-pressure container has reached a preset value.
器内温度との差を検出して昇温量を求め、該昇温量が予
め設定された値に到達した事を検知する事により、前記
結晶生成量の所定量到達の検知を行う第１請求項に記載
の圧力晶析方法。(3) Detect the difference between the temperature of the raw material fed into the high-pressure container and the temperature inside the high-pressure container after pressurization to determine the amount of temperature increase, and detect when the amount of temperature increase has reached a preset value. 2. The pressure crystallization method according to claim 1, wherein said method detects whether said crystal formation amount reaches a predetermined amount.
のピストンの変移を検出し、該変移が予め設定された値
に到達した事を検知する事により、前記結晶生成量の所
定量到達の検知を行う第１請求項に記載の圧力晶析方法
。(4) By using a high-pressure container having a pressurizing piston, detecting the displacement of the piston after pressurization, and detecting that the displacement has reached a preset value, the predetermined amount of crystal formation is reached. The pressure crystallization method according to claim 1, wherein the pressure crystallization method detects.
設定された値に到達した事を検知する事により、前記結
晶生成量の所定量到達の検知を行う第４請求項に記載の
圧力晶析方法。(5) The pressure according to claim 4, wherein reaching the predetermined amount of crystal formation is detected by detecting that the displacement of the piston after reaching the predetermined pressure has reached a preset value. Crystallization method.
間該圧力に保持し、次いで前記固液分離を開始すること
を特徴とする第１請求項又は第３請求項に記載の圧力晶
析方法。(6) After reaching the predetermined pressure, the pressure is maintained at the pressure for a predetermined period of time, and then the solid-liquid separation is started. Analysis method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15869488A JPH026801A (en) | 1988-06-27 | 1988-06-27 | Pressure crystallization method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP15869488A JPH026801A (en) | 1988-06-27 | 1988-06-27 | Pressure crystallization method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH026801A true JPH026801A (en) | 1990-01-11 |
| JPH0356761B2 JPH0356761B2 (en) | 1991-08-29 |
Family
ID=15677314
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP15869488A Granted JPH026801A (en) | 1988-06-27 | 1988-06-27 | Pressure crystallization method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH026801A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000220605A (en) * | 1999-01-26 | 2000-08-08 | Mannesmann Rexroth Sa | Hydraulic type direction control valve |
-
1988
- 1988-06-27 JP JP15869488A patent/JPH026801A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000220605A (en) * | 1999-01-26 | 2000-08-08 | Mannesmann Rexroth Sa | Hydraulic type direction control valve |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0356761B2 (en) | 1991-08-29 |
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