JP2849142B2 - Pressure crystallization equipment - Google Patents
Pressure crystallization equipmentInfo
- Publication number
- JP2849142B2 JP2849142B2 JP1650390A JP1650390A JP2849142B2 JP 2849142 B2 JP2849142 B2 JP 2849142B2 JP 1650390 A JP1650390 A JP 1650390A JP 1650390 A JP1650390 A JP 1650390A JP 2849142 B2 JP2849142 B2 JP 2849142B2
- Authority
- JP
- Japan
- Prior art keywords
- pressure
- piston
- valve
- exhaust pipe
- liquid
- 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 34
- 230000008025 crystallization Effects 0.000 title claims description 32
- 239000007788 liquid Substances 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 4
- 230000000149 penetrating effect Effects 0.000 claims description 2
- 239000000047 product Substances 0.000 description 16
- 239000002994 raw material Substances 0.000 description 15
- 239000007791 liquid phase Substances 0.000 description 7
- 230000007423 decrease Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000012265 solid product Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229930003836 cresol Natural products 0.000 description 1
- 238000007599 discharging 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
- 239000012530 fluid Substances 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 210000004243 sweat Anatomy 0.000 description 1
- -1 that is Substances 0.000 description 1
- 238000005406 washing Methods 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、圧力晶析装置に関し、詳細には、特定成分
を含む２種以上の成分からなる混合物について特定成分
を圧力下で晶析させ、分離する圧力晶析法に使用する圧
力晶析装置に関する。Description: FIELD OF THE INVENTION The present invention relates to a pressure crystallization apparatus, and more specifically, to crystallize a specific component under pressure from a mixture of two or more components including the specific component. And a pressure crystallization apparatus used in a pressure crystallization method for separating.
（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。(Prior art) Pressure crystallization has great potential for application to raw material systems that are difficult to separate by conventional distillation and cooling crystallization, and that high-purity products are easily obtained. This is a separation and purification technique that has attracted a great deal of attention in recent years as the chemical industry has become finer, because of its easy yield and low energy consumption.
従来の圧力晶析法と装置の代表例を第３図に示し、以
下説明する。内周壁に筒状フィルタ（２）を配した耐圧
性筒体（１）の下開口部に蓋体（３）を密嵌し、上開口
部からピストン（４）を嵌入して形成した高圧容器
（９）内の晶析室（８）に、原料供給ポンプP,給液弁V1
を介して予備晶析缶Ｄが原料供給管（５）で連結され、
又、フィルタ（２）背面下部に連通する排液口（６）に
排液弁V2及び減圧ノズルＮが管接続され、さらに排液タ
ンクＴが連結されている。FIG. 3 shows a typical example of a conventional pressure crystallization method and apparatus, which will be described below. A high-pressure container formed by tightly fitting a lid (3) into a lower opening of a pressure-resistant cylinder (1) having a cylindrical filter (2) disposed on an inner peripheral wall, and fitting a piston (4) through an upper opening. In the crystallization chamber (8) in (9), the raw material supply pump P and the supply valve V 1
And the preliminary crystallizer D is connected by a raw material supply pipe (5),
The filter (2) drain valve V 2 and vacuum nozzle N to the liquid discharge port (6) communicating with the lower back is a tube connected are further connected drainage tank T is.
前記ピストン（４）には、その下先端部から内部を貫
通し外部に連通する給液・排気用の排気管（10）が設け
られ、ピストン（４）外部に位置する排気管（10）の途
中には給液検知器（11）及び開閉弁V3が設けられてい
る。The piston (4) is provided with an exhaust pipe (10) for liquid supply and exhaust that penetrates the inside from the lower end thereof and communicates with the outside, and the exhaust pipe (10) located outside the piston (4) is provided. supply fluid detector (11) and the on-off valve V 3 is provided midway.
上記装置により圧力晶析するに際しては、先ず、原料
を予備晶析缶Ｄで冷却して圧力晶析のための種結晶を生
成せしめた後、弁V1,V3を開き原料供給管（５）から晶
析室（８）に注入し、充満した事を給液検知器（11）に
より検知すると、弁V1,V3を閉じピストン（４）より晶
析室（８）内の原料を所定圧力に加圧し、特定物質を晶
析させ、所定の固液共存状態にする。次に、固液分離す
るため、直ちに弁V2を開き、前記圧力を維持した状態で
ピストン（４）を下降させ、フィルタ（２），弁V2,減
圧ノズルＮを介して排液管（14）により液相を排液タン
クＴに排出する。通常の場合、更に加圧圧搾して結晶粒
間の残留液体を絞り出し、排出する。引き続きピストン
（４）を下降させると、塊状固体製品に成形され、その
後晶析室（８）の液相圧力が次第に低下し、結晶表面が
部分的に融解して所謂発汗洗浄され、塊状固体製品の精
製がなされる。When pressure crystallization is performed by the above apparatus, first, the raw material is cooled in a preliminary crystallizer D to generate a seed crystal for pressure crystallization, and then the valves V 1 and V 3 are opened to open the raw material supply pipe (5). ) Into the crystallization chamber (8), and when the filling is detected by the liquid supply detector (11), the valves V 1 and V 3 are closed, and the raw material in the crystallization chamber (8) is discharged from the piston (4). By pressurizing to a predetermined pressure, a specific substance is crystallized and brought into a predetermined solid-liquid coexistence state. Then, to solid-liquid separation immediately open the valve V 2, to lower the piston (4) while maintaining the pressure, the filter (2), the valve V 2, the drainage tube through the vacuum nozzle N ( The liquid phase is discharged to the drain tank T according to 14). In a normal case, the liquid remaining between the crystal grains is further squeezed out by pressing under pressure and discharged. Subsequently, when the piston (4) is lowered, it is formed into a lump solid product, and thereafter, the liquid phase pressure in the crystallization chamber (8) gradually decreases, and the crystal surface partially melts, so-called sweat washing is performed, and the lump solid product is formed. Is purified.
上記排出する液相圧が所定圧に低下すると、ピストン
（４）及び筒体（１）を上昇させた後、プッシャー
（７）等により蓋（３）上の固体製品を取り出す。その
後は筒体（１）を下降して蓋（３）に嵌合し、以下原料
の注入工程に戻り、同様の工程を繰り返し、製品を生産
する。When the discharged liquid phase pressure decreases to a predetermined pressure, the piston (4) and the cylinder (1) are raised, and then the solid product on the lid (3) is taken out by a pusher (7) or the like. Thereafter, the cylindrical body (1) is lowered and fitted to the lid (3). Thereafter, the process returns to the raw material injection step, and the same steps are repeated to produce a product.
（発明が解決しようとする課題） ところが、前記ピストン（４）先端部から開閉弁V3ま
での排気管（10）内の液相は前記液相排出工程で排出さ
れず、該工程後も該排気管（10）内に残留しているの
で、該残留液が前記ピストン（４）及び筒体（１）の上
昇及び製品取出し時に製品表面に付着する。該残留液は
特定物質以外の成分即ち不純物を多く含有している。従
って、該残留液付着により製品純度が損なわれる。これ
は、高純度製品に分離して得ることを目的とする圧力晶
析において極めて深刻な問題点である。(Problem to be Solved by the Invention) However, the piston (4) exhaust pipe from the tip to the on-off valve V 3 (10) in the liquid phase is not ejected by the liquid phase discharge process, after the process is also the Since the residual liquid remains in the exhaust pipe (10), the residual liquid adheres to the surface of the product when the piston (4) and the cylinder (1) are lifted and the product is taken out. The residual liquid contains a large amount of components other than the specific substance, that is, impurities. Therefore, the product purity is impaired by the adhesion of the residual liquid. This is a very serious problem in pressure crystallization aimed at separating and obtaining high-purity products.
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、排気管内の残留液の付着による製品純度の低下
を大幅に軽減し得る圧力晶析装置を提供しようとするも
のである。The present invention has been made in view of such circumstances, and has as its object to solve the above-mentioned problems and to significantly reduce the reduction in product purity due to the adhesion of residual liquid in the exhaust pipe. It is an object of the present invention to provide a pressure crystallization apparatus capable of reducing the pressure.
（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、本発明に係る圧力晶析
装置は次のような構成としている。(Means for Solving the Problems) In order to achieve the above object, a pressure crystallization apparatus according to the present invention has the following configuration.
即ち、請求項１に記載の装置は、耐圧性筒体の下開口
部に蓋体を密嵌し、該筒体の上開口部からピストンを嵌
入してなる高圧容器と、該容器内への混合物供給手段
と、該容器に接続された液排出手段とを有しており、前
記ピストンの下先端部から内部を貫通し外部に連通する
排気管を設け、該排気管に開閉弁及び給液検知器を設け
た圧力晶析装置において、前記開閉弁をピストンの下先
端部の近傍に配したことを特徴とする圧力晶析装置であ
る。That is, the device according to claim 1 is a high-pressure container in which a lid is closely fitted to a lower opening of a pressure-resistant cylinder, and a piston is fitted from an upper opening of the cylinder, An exhaust pipe having a mixture supply means and a liquid discharge means connected to the container, and an exhaust pipe penetrating through the inside from the lower end of the piston and communicating with the outside; A pressure crystallization apparatus provided with a detector, wherein the on-off valve is disposed near a lower end of a piston.
請求項２に記載の装置は、前記給液検知器をピストン
の下先端部の近傍に配した請求項１に記載の圧力晶析装
置である。An apparatus according to a second aspect is the pressure crystallization apparatus according to the first aspect, wherein the liquid supply detector is disposed near a lower end of the piston.
（作 用） 本発明に係る圧力晶析装置は、前記の如く、ピストン
の下先端部から内部を貫通し外部に連通する排気管の開
閉弁をピストンの下先端部の近傍に配しているので、該
ピストン先端部から開閉弁までの排気管内の容積は極め
て小さい。そのため、該排気管内において液相排出工程
で排出されず、残留する液の量は極めて少く、その結果
ピストン及び筒体の上昇及び製品取出し時に製品表面に
付着する残留液は、前述の従来装置の場合に比し、極め
て少量である。従って、排気管内の残留液付着による製
品純度の低下を大幅に軽減し得る。(Operation) As described above, in the pressure crystallization apparatus according to the present invention, the on-off valve of the exhaust pipe that penetrates the inside from the lower end of the piston and communicates with the outside is arranged near the lower end of the piston. Therefore, the volume in the exhaust pipe from the tip of the piston to the on-off valve is extremely small. Therefore, the amount of liquid remaining in the exhaust pipe during the liquid phase discharging step and remaining is extremely small. It is extremely small compared to the case. Therefore, it is possible to greatly reduce a decrease in product purity due to adhesion of the residual liquid in the exhaust pipe.
上記排気管に設ける給液検知器の配置位置は限定され
ず、ピストン外部に位置されてもよく、前記開閉弁の近
傍に位置させることもできる。前者の場合、少なくとも
開閉弁から給液検知器までの排気管内の原料は圧力晶析
されず、回収する必要があり、不経済である。後者の場
合は上記の如き排気管内原料の量が少ない。従って、給
液検知器は前記開閉弁の近傍に設けることが望ましい。
特に、ピストン先端部から前記開閉弁までの間に設ける
と、上記の如き排気管内原料の量を皆無にし得るので良
い。The position of the liquid supply detector provided in the exhaust pipe is not limited, and may be located outside the piston, or may be located near the on-off valve. In the former case, at least the raw material in the exhaust pipe from the on-off valve to the liquid supply detector is not pressure-crystallized and must be recovered, which is uneconomical. In the latter case, the amount of the raw material in the exhaust pipe as described above is small. Therefore, it is desirable to provide the liquid supply detector near the on-off valve.
In particular, when provided between the tip of the piston and the on-off valve, the amount of the raw material in the exhaust pipe as described above can be completely eliminated.
（実施例） 実施例１ 実施例１に係る圧力晶析装置を第１図に示す。該装置
は、排気管（10）の開閉弁（12）をピストン（４）の下
先端部の近傍に配したものであり、その他の点は第３図
に示したものと同様である。(Example) Example 1 A pressure crystallization apparatus according to Example 1 is shown in FIG. In this device, an on-off valve (12) of an exhaust pipe (10) is arranged near a lower end of a piston (4), and the other points are the same as those shown in FIG.
上記装置を用い、下記の如く圧力晶析を実施した。先
ず、原料の混合物（Ｐ−成分80％,m−成分20％のクレゾ
ール混合溶液）を予備晶析缶Ｄで冷却して種結晶を生成
せしめた後、弁V1及び排気管（10）の開閉弁（12）を開
き、原料供給管（５）から晶析室（８）に注入し、充満
した事を給液検知器（11）により検知すると同時に、弁
V1及び開閉弁（12）を閉じた。その直後、ピストン
（４）を下降して所定圧力まで加圧した。該圧力は、12
00、1500及び1800気圧の３種類に変化させた。尚、上記
加圧に並行して開閉弁（12）から給液検知器（11）まで
の排気管（10）内の原料の回収も行った。Pressure crystallization was performed as described below using the above apparatus. First, a mixture of starting material after yielding seed crystal and cooled (P- component 80%, m-content of 20% cresol mixed solution) in the pre-crystallizer D, valves V 1 and an exhaust pipe (10) Open the on-off valve (12), inject it from the raw material supply pipe (5) into the crystallization chamber (8), and when the filling is detected by the liquid supply detector (11),
Closing the V 1 and on-off valve (12). Immediately thereafter, the piston (4) was lowered and pressurized to a predetermined pressure. The pressure is 12
The pressure was changed to three types: 00, 1500 and 1800 atm. In parallel with the pressurization, raw materials in the exhaust pipe (10) from the on-off valve (12) to the liquid supply detector (11) were also collected.
次いで、直ちに排液弁V2を開き、上記圧力を維持した
状態でピストン（４）を下降させ、フィルタ（２）、弁
V2及び減圧ノズルＮを介して晶析室（８）内の液相を排
液タンクＴに排出した。続いて、圧搾して残留液を絞り
出し、排液した。該排液後、ピストン（４）及び筒体
（１）を上昇させ、蓋（３）上の固体製品を取り出し
た。その後は筒体（１）を下降して蓋（３）に嵌合し、
以下原料の注入工程に戻り、同様の工程を繰り返し、製
品を生産した。Then, immediately open the drain valve V 2, to lower the piston (4) while maintaining the pressure, the filter (2), the valve
Through the V 2 and vacuum nozzle N was discharged liquid phase in the crystallization chamber (8) to the drainage tank T. Subsequently, the remaining liquid was squeezed out by pressing and drained. After the drainage, the piston (4) and the cylinder (1) were raised, and the solid product on the lid (3) was taken out. After that, the cylinder (1) is lowered and fitted to the lid (3),
Thereafter, the process returns to the raw material injection step, and the same steps are repeated to produce a product.
その結果、得られた製品の純度を、従来装置を使用し
前記と同様の圧力晶析をして得られた製品純度と共に第
１表に示す。いづれの晶析加圧力の場合も、本発明に係
る装置を使用した実施例１の場合は、従来装置を使用し
た場合に比し、製品純度が高いことが判る。これは、排
気管（10）の残留液付着による製品純度の低下が大幅に
軽減されたためである。As a result, the purity of the obtained product is shown in Table 1 together with the product purity obtained by the same pressure crystallization as described above using a conventional apparatus. Regardless of the crystallization pressure, it can be seen that the product purity is higher in Example 1 using the apparatus according to the present invention than in the case of using the conventional apparatus. This is because the decrease in the purity of the product due to the adhesion of the residual liquid to the exhaust pipe (10) has been greatly reduced.
実施例２ 実施例２に係る圧力晶析装置を第２図に示す。該装置
は、排気管（10）の給液検知器（13）をピストン（４）
の下先端部と開閉弁（12）との間に配置したものであ
り、その他の点は実施例１に係る圧力晶析装置と 同様である。該装置を用い、実施例１の場合と同様の圧
力晶析を実施した。その結果、実施例１の場合と同様、
従来装置を使用した場合に比し、製品純度が高いことが
確認された。尚、開閉弁（12）から給液検知器（11）ま
での排気管（10）内の原料の量は皆無に等しく、該原料
回収の所要時間は実施例１の場合に比し、短縮された。Example 2 FIG. 2 shows a pressure crystallization apparatus according to Example 2. The device connects the liquid supply detector (13) of the exhaust pipe (10) to the piston (4).
The pressure crystallization apparatus according to the first embodiment is disposed between the lower tip and the on-off valve (12). The same is true. Pressure crystallization was performed in the same manner as in Example 1 using this apparatus. As a result, similar to the first embodiment,
It was confirmed that the product purity was higher than when using the conventional device. In addition, the amount of the raw material in the exhaust pipe (10) from the on-off valve (12) to the liquid supply detector (11) is equal to nothing, and the time required for collecting the raw material is shorter than that in the first embodiment. Was.
（発明の効果） 本発明に係る圧力晶析装置によれば、給液・排気用の
排気管内の残留液の付着による製品純度の低下を大幅に
軽減し得るようになる。そのため、従来装置による場合
に比し、製品純度を向上し得るようになる。(Effects of the Invention) According to the pressure crystallization apparatus according to the present invention, it is possible to greatly reduce a decrease in product purity due to adhesion of a residual liquid in an exhaust pipe for supplying and exhausting liquid. Therefore, the product purity can be improved as compared with the case using the conventional apparatus.
第１図は実施例１に係る圧力晶析装置の概要を示す側断
面図、第２図は実施例２に係る圧力晶析装置の概要を示
す側断面図、第３図は従来の圧力装置の代表例を示す側
断面図である。 （１）……耐圧性筒体、（２）……筒状フィルタ （３）……蓋体、（４）……ピストン （５）……原料供給管、（６）……排液口 （７）……プッシヤー、（８）……晶析室 （９）……高圧容器、（10）……排気管 （11）……給液検知器、（12）……開閉弁 （13）……給液検知器、（14）……排液管 Ｐ……原料供給ポンプ、Ｄ……予備晶析缶 Ｎ……減圧ノズル、Ｔ……排液タンク V1……給液弁、V2……排液弁 V3……開閉弁1 is a side sectional view showing an outline of a pressure crystallization apparatus according to Embodiment 1, FIG. 2 is a side sectional view showing an outline of a pressure crystallization apparatus according to Embodiment 2, and FIG. 3 is a conventional pressure apparatus. It is a sectional side view which shows the typical example. (1) ... pressure-resistant cylinder, (2) ... tubular filter (3) ... lid, (4) ... piston (5) ... material supply pipe, (6) ... drain port ( 7) Pusher, (8) Crystallization chamber (9) High-pressure vessel, (10) Exhaust pipe (11) Liquid supply detector, (12) On-off valve (13) ... Supply detector, (14) ... Drain pipe P ... Material supply pump, D ... Preliminary crystallizer N ... Negative pressure nozzle, T ... Drain tank V 1 ... Supply valve, V 2 …… Drain valve V 3 …… On-off valve
───────────────────────────────────────────────────── フロントページの続き (72)発明者 高田 俊助 兵庫県神戸市灘区篠原伯母野山町２―３ ―１ (56)参考文献 特開 平３−258301（ＪＰ，Ａ) 特開 昭63−209703（ＪＰ，Ａ) (58)調査した分野(Int.Cl.6，ＤＢ名) B01D 9/02──────────────────────────────────────────────────続 き Continuation of the front page (72) Inventor Shunsuke Takada 2-3-1 Shinohara Akiminoyama-cho, Nada-ku, Kobe City, Hyogo Prefecture (56) References JP-A-3-258301 (JP, A) JP-A-63- 209703 (JP, A) (58) Field surveyed (Int. Cl. 6 , DB name) B01D 9/02
Claims (2)
筒体の上開口部からピストンを嵌入してなる高圧容器
と、該容器内への混合物供給手段と、該容器に接続され
た液排出手段とを有しており、前記ピストンの下先端部
から内部を貫通し外部に連通する排気管を設け、該排気
管に開閉弁及び給液検知器を設けた圧力晶析装置におい
て、前記開閉弁をピストンの下先端部の近傍に配したこ
とを特徴とする圧力晶析装置。1. A high-pressure container having a lid tightly fitted to a lower opening of a pressure-resistant cylinder, a piston inserted from an upper opening of the cylinder, a means for supplying a mixture into the container, A liquid discharge means connected to the container, an exhaust pipe penetrating through the inside from the lower end of the piston and communicating with the outside, and an open / close valve and a liquid supply detector provided on the exhaust pipe. A pressure crystallization apparatus, wherein the on-off valve is arranged near a lower end of a piston.
傍に配した請求項１に記載の圧力晶析装置。2. The pressure crystallization apparatus according to claim 1, wherein said liquid supply detector is arranged near a lower end of a piston.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1650390A JP2849142B2 (en) | 1990-01-25 | 1990-01-25 | Pressure crystallization equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1650390A JP2849142B2 (en) | 1990-01-25 | 1990-01-25 | Pressure crystallization equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03221102A JPH03221102A (en) | 1991-09-30 |
| JP2849142B2 true JP2849142B2 (en) | 1999-01-20 |
Family
ID=11918079
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1650390A Expired - Fee Related JP2849142B2 (en) | 1990-01-25 | 1990-01-25 | Pressure crystallization equipment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2849142B2 (en) |
-
1990
- 1990-01-25 JP JP1650390A patent/JP2849142B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03221102A (en) | 1991-09-30 |
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| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |