JP5941380B2 - Distillation tower with self-heating and heat insulation effect - Google Patents

Distillation tower with self-heating and heat insulation effect Download PDF

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JP5941380B2
JP5941380B2 JP2012196203A JP2012196203A JP5941380B2 JP 5941380 B2 JP5941380 B2 JP 5941380B2 JP 2012196203 A JP2012196203 A JP 2012196203A JP 2012196203 A JP2012196203 A JP 2012196203A JP 5941380 B2 JP5941380 B2 JP 5941380B2
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distillation
distillation column
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outlet pipe
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弥太郎 桐山
弥太郎 桐山
時男 桐山
時男 桐山
啓祐 板倉
啓祐 板倉
加藤 大介
大介 加藤
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有限会社桐山製作所
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Description

本発明は、蒸留塔に関する。さらに詳しくは、例えば、化学研究、石油工業、薬学その他の各種分野の蒸留技術において、液体混合物を加熱蒸発させて成分分離する際等に使用する蒸留塔に関する。   The present invention relates to a distillation column. More specifically, for example, the present invention relates to a distillation column used for separating components by heating and evaporating a liquid mixture in distillation techniques in various fields such as chemical research, petroleum industry, pharmacy and the like.

蒸留塔は、その構造等により、例えば充填塔、オルダーショウ塔、シープ塔、棚段塔、ビーグロー塔、ヘンベル塔、シュナイダー塔、その他多数の形式のものがある(例えば、非特許文献1等参照)。   Depending on the structure of the distillation tower, there are, for example, a packed tower, an Oldershaw tower, a sheep tower, a plate tower, a bee glow tower, a Hembell tower, a Schneider tower, and many other types (see, for example, Non-Patent Document 1). .

蒸留塔の性能を高めるためには、上昇蒸気と塔高(長)の各位置で自然に冷却還流する液体との気液接触が必要であり、その熱交換の多少(多い少ない)により性能に差が生じる。塔長を長くすれば熱交換が多く行なわれ低沸点成分が多くなるが、熱の放出、逸散が多くなるため、実際は塔長に限度がある。   In order to improve the performance of the distillation tower, it is necessary to make gas-liquid contact between the rising steam and the liquid that naturally cools and recirculates at each position of the tower height (long). There is a difference. Increasing the column length increases heat exchange and increases the low-boiling components. However, since the release and dissipation of heat increase, the column length is actually limited.

そこで、電熱線やリボンヒーター等で蒸留塔(塔内を上昇する蒸気)を人為的に加熱保温する方法が一般的に採用されているが、混合留分の上昇と最適の加熱温度を得て保温を行なうことは対象試料(蒸留対象の液体混合物)の多様性により、先づ不可能に近い。   Therefore, a method of artificially heating and maintaining the distillation tower (steam rising in the tower) with a heating wire, ribbon heater, etc. is generally adopted, but the rise of the mixed fraction and the optimum heating temperature are obtained. It is almost impossible to keep the temperature first because of the diversity of the target sample (liquid mixture to be distilled).

本発明者らは、蒸留塔を上述した最適な温度で加熱保温(与熱保温)することにより、分留効果に多大な影響をもたらすものと確信した。しかるに、上記技術は未だ開発されていないのが現状である。   The inventors of the present invention have convinced that heating and maintaining the distillation column at the above-described optimum temperature (heat-retaining temperature) has a great influence on the fractionation effect. However, the present technology has not been developed yet.

丸善株式会社発行の科学大辞典Science Dictionary published by Maruzen Co., Ltd.

本発明は上記のような実情に鑑み、蒸留塔の前記与熱保温が分留効果に多大な影響があるとの技術思想(理念)に基づき自然に、人為的技術によらないで所謂インテリジェントな与熱保温の効果を簡単な原理的構成により蒸留塔に具備させ、蒸留性能を大巾に向上し得る蒸留塔を提供することを目的とするものである。   In view of the above situation, the present invention is based on the technical idea (philosophy) that the heating and heat insulation of the distillation column has a great influence on the fractional distillation effect, so-called intelligently without relying on artificial techniques. An object of the present invention is to provide a distillation column that can provide a distillation column with the effect of heat insulation by a simple principle configuration and can greatly improve the distillation performance.

上記目的を達成するため、本発明者らは、試験、研究を継続して行なった結果、所期の目的を達成した発明を完成したので、ここに提案する。   In order to achieve the above-mentioned object, the present inventors have conducted an examination and research, and as a result, completed the invention that has achieved the intended object, and proposes it here.

即ち、本発明のうち、1つの発明(第1の発明)は、蒸留塔において、
蒸留塔本体と、前記塔本体の外周面の略全域との間に略円筒状の空隙部を形成して設けた保温用の外筒体とを備え、
蒸留釜内の液体混合物から発生する蒸発蒸気を前記塔本体及び前記空隙部へ導入し、前記空隙部へ導入する前記蒸気により、前記空隙部に、前記塔本体を熱保温する自己与熱保温効果を具備させるように構成したことを特徴とする。
That is, of the present invention, one invention (first invention) is a distillation column,
A distillation column main body, and an outer cylinder for heat insulation provided by forming a substantially cylindrical void between the entire outer peripheral surface of the column main body,
Evaporation vapor generated from the liquid mixture of the distillation still was introduced into the tower body and the gap portion, by the steam introduced into the gap portion, the gap portion, a self Azukanetsu incubated for pressurizing the heat insulation of the tower body It is characterized by having an effect.

本発明は上記のように蒸留釜内の液体混合物そのものの蒸発蒸気を塔本体及び前記空隙部へ導入し、前記液体混合物の蒸発蒸気そのもので塔本体を与熱保温(加熱保温)するように構成されている。前記同一液体混合物での上昇蒸気は、当然複数種の混合液であるから、塔本体の下部側では混合液中の高沸点物蒸気、また、塔本体の上部側は低沸点物蒸気により加熱保温され、この温度勾配は両者ともに同一成分の液体混合物の蒸発蒸気であるため、塔本体内を上昇する蒸留対象の液体混合物の蒸発蒸気に近似の温度分布を与える。これにより、過加熱、フラッディング、低温による上昇困難等を防止して分留を行なうことができる。 The present invention is configured to introduce the vaporized vapor of the liquid mixture itself in the distillation kettle into the tower body and the gap as described above, and to heat and maintain the tower body with the vaporized vapor itself of the liquid mixture (heated and kept warm). Has been. Since the rising vapor in the same liquid mixture is naturally a mixture of a plurality of types, the high boiling point vapor in the mixed solution is heated on the lower side of the tower body, and the upper side of the tower body is heated and maintained by the low boiling point vapor. Since both of these temperature gradients are vapors of the liquid mixture of the same component, an approximate temperature distribution is given to the vapors of the liquid mixture to be distilled that rises in the column body. Thereby, fractional distillation can be performed while preventing overheating, flooding, difficulty in rising due to low temperature, and the like.

なお、本発明において、「蒸留塔」の用語は、分留塔、精留塔、蒸留管、分留管及び精留管と同義語として用いられている。また、「液体混合物」には、「混合溶液」も含まれる。さらにまた、「蒸留釜」には、蒸留フラスコなども含まれる。   In the present invention, the term “distillation column” is used as a synonym for fractionation column, rectification column, distillation tube, fractionation tube, and rectification tube. The “liquid mixture” also includes “mixed solution”. Furthermore, the “distilling kettle” includes a distillation flask and the like.

本発明は、充填塔、オルダーショウ塔、シープ塔、棚段塔、ビーグロー塔(管)、ヘンベル塔(管)、シュナイダー塔(管)、その他各種形式の工業用及び実験用の蒸留塔に適用可能である。
また、常圧蒸留,減圧(真空)蒸留及び加圧蒸留の全ての蒸留操作に適用できる。
The present invention can be applied to packed towers, Oldershaw towers, sheep towers, plate towers, bee glow towers (tubes), Hembel towers (tubes), Schneider towers (tubes), and other various types of industrial and experimental distillation columns. It is.
Further, it can be applied to all distillation operations such as atmospheric distillation, reduced pressure (vacuum) distillation and pressure distillation.

本発明の他の1つの発明(第2の発明)は、第1の発明の蒸留塔において、前記外筒体の外側に保温用真空ジャケットその他の保温手段を設けたことを特徴とする。   Another invention of the present invention (second invention) is characterized in that, in the distillation column of the first invention, a heat insulating vacuum jacket or other heat retaining means is provided outside the outer cylindrical body.

本発明の他の1つの発明(第3の発明)は、第1又は第2の発明の蒸留塔において、前記空隙部と連通させて前記外筒体の上端部から上方部側へ向けて突出させて設けた蒸気導出管部と、
前記導出管部と連通させて前記導出管部の上端部に設けた冷却器とを備えていることを特徴とする。
Another invention of the present invention (third invention) is the distillation tower according to the first or second invention, wherein it projects from the upper end portion of the outer cylindrical body toward the upper portion side in communication with the gap portion. A steam outlet pipe provided, and
And a cooler provided at the upper end of the outlet pipe portion in communication with the outlet pipe portion.

本発明の他の1つの発明(第4の発明)は、第1又は第2の発明の蒸留塔において、前記空隙部と連通させて前記外筒部の上端部から上方部側へ向けて突出させて設けた蒸気導出管部と、
前記導出管部と連通させて前記導出管部の上端部に設けた冷却器と、
一端部の先端を前記導出管部と連通させて前記導出管部に気密性を保持して固定すると共に他端部の先端を前記空隙部と連通させて前記外筒体の所望の部位に気密性を保持して固定して設けた還流用管路とを備えていることを特徴とする。
Another invention of the present invention (fourth invention) is the distillation tower according to the first or second invention, wherein it projects from the upper end portion of the outer cylinder portion toward the upper portion side in communication with the gap portion. A steam outlet pipe provided, and
A cooler provided at the upper end of the outlet pipe portion in communication with the outlet pipe portion;
The tip of one end is communicated with the lead-out tube and is fixed to the lead-out tube while maintaining airtightness, and the tip of the other end is communicated with the gap and airtight to a desired part of the outer cylinder. And a reflux conduit that is fixed while maintaining the property.

本発明の他の1つの発明(第5の発明)は、第4の発明の蒸留塔において、前記還流用管路は、前記他端部にU字状管路を備えていることを特徴とする。   Another invention of the present invention (fifth invention) is characterized in that, in the distillation column of the fourth invention, the reflux pipe has a U-shaped pipe at the other end. To do.

本発明によれば、次のような作用効果を奏する。
(1)蒸留塔本体の外側面から加熱保温などの面倒な操作を必要とせず、外筒体の蒸気に起因する自己与熱保温効果により、蒸留塔自身で保温機能が働き、理論段数50段以上の高性能の精密蒸留が達成できる自己制御可能な蒸留塔を提供できる。
(2)フラッデイング、過加熱、及び低温による上昇困難等を防止することができる。
(3)沸点が極めて接近した化合物、例えば、香料産業などで重要なゲラニオール(沸点230℃)とネロール(沸点227℃)などテルペン化合物の異性体の精密分留等にも最適な蒸留機能を発揮する。
(4)第3及び第4の発明によれば、上記諸効果に加え、前記空隙部へ導入された蒸発蒸気が上昇し易くなる。したがって、分留(蒸留)性能を一層向上させることができる。
According to the present invention, the following operational effects can be obtained.
(1) There is no need for troublesome operations such as heat insulation from the outer surface of the distillation column main body, and the heat retention function works by the distillation column itself due to the self-heating heat retention effect caused by the steam of the outer cylinder, and the theoretical number of plates is 50 A self-controllable distillation column capable of achieving the above high-performance precision distillation can be provided.
(2) It is possible to prevent flooding, overheating, difficulty in rising due to low temperature, and the like.
(3) Optimal distillation function for precision fractionation of isomers of terpene compounds such as geraniol (boiling point 230 ° C) and nerol (boiling point 227 ° C), which are important in the perfume industry, such as geraniol (boiling point 227 ° C). To do.
(4) According to the third and fourth inventions, in addition to the above effects, the evaporated vapor introduced into the gap portion is likely to rise. Therefore, fractional distillation (distillation) performance can be further improved.

本発明の一実施形態の蒸留塔の構成を概略的に示す図であって、同図(a)は縦断面図、同図(b)は同図(a)のA−A線拡大断面図である。BRIEF DESCRIPTION OF THE DRAWINGS It is a figure which shows schematically the structure of the distillation tower of one Embodiment of this invention, Comprising: The same figure (a) is a longitudinal cross-sectional view, The same figure (b) is the AA line expanded sectional view of the same figure (a). It is. 前記蒸留塔の一部を拡大し、使用状態及び作用を示す説明図である。It is explanatory drawing which expands a part of said distillation tower and shows a use condition and an effect | action. 前記蒸留塔を用いて構成した蒸留装置の一例の構成を概略的に示す説明図である。It is explanatory drawing which shows roughly the structure of an example of the distillation apparatus comprised using the said distillation tower. 前記蒸留塔を用いて構成した理論段数測定用の蒸留装置を概略的に示す説明図である。It is explanatory drawing which shows roughly the distillation apparatus for the theoretical plate number measurement comprised using the said distillation tower. 本発明の他の実施形態の蒸留塔の要部の構成を概略的に示す縦断面図である。It is a longitudinal cross-sectional view which shows schematically the structure of the principal part of the distillation tower of other embodiment of this invention. 本発明のさらに他の実施形態の蒸留塔の構成を概略的に示す縦断面図である。It is a longitudinal cross-sectional view which shows schematically the structure of the distillation tower of other embodiment of this invention. 本発明のさらに他の実施形態の蒸留塔の構成を概略的に示す図であって、同図(a)は縦断面図、同図(b)は同図(a)の前記蒸留塔に採用した冷却器を拡大し、その構成を概略的に示す縦断面図である。It is a figure which shows schematically the structure of the distillation column of further another embodiment of this invention, Comprising: The same figure (a) is a longitudinal cross-sectional view, The same figure (b) is employ | adopted as the said distillation tower of the same figure (a). It is a longitudinal cross-sectional view which expands the made cooler and shows the structure roughly. 本発明のさらに他の実施形態の蒸留塔の構成を概略的に示す図であって、同図(a)は縦断面図、同図(b)は同図(a)の蒸留塔の上端部側の一部を拡大し、その構成を概略的に示す縦断面説明図、同図(c)は同じく下端部側の一端を拡大し、その構成を概略的に示す縦断面説明図である。It is a figure which shows schematically the structure of the distillation column of further another embodiment of this invention, Comprising: The same figure (a) is a longitudinal cross-sectional view, The same figure (b) is the upper end part of the distillation tower of the same figure (a). FIG. 4C is a longitudinal cross-sectional explanatory view schematically showing the configuration of the lower end portion side, with a part of the side enlarged and schematically showing the configuration. FIG.

以下、図面を参照して本発明の実施形態の一例について説明する。   Hereinafter, an example of an embodiment of the present invention will be described with reference to the drawings.

図1は本発明の一実施形態(実施形態1)を示す。実施形態1は、本発明の蒸留塔を実験用の蒸留塔に適用した一例を示す。   FIG. 1 shows an embodiment (Embodiment 1) of the present invention. Embodiment 1 shows an example in which the distillation column of the present invention is applied to an experimental distillation column.

実施形態1の蒸留塔100は充填塔で構成され、蒸留塔本体1と、保温用の外筒体2とを備える。外筒体2は、塔本体1の外周面の略全域との間に略円筒状の空隙部20を形成して設けてある。   The distillation column 100 of Embodiment 1 is constituted by a packed column, and includes a distillation column main body 1 and an outer cylinder 2 for heat insulation. The outer cylindrical body 2 is provided with a substantially cylindrical void 20 formed between substantially the entire outer peripheral surface of the tower body 1.

塔本体1は下端を開口し、上端部にジョイント口管10(メスジョイント)を備える。実施形態1の塔本体1は開口下端に充填物受け用の円錐状金網11を備え、塔本体1内には蒸留用充填物12が充填されている。   The tower main body 1 has a lower end and a joint mouth pipe 10 (female joint) at the upper end. The tower main body 1 of Embodiment 1 is provided with a conical metal mesh 11 for receiving a packing at the lower end of the opening, and the tower main body 1 is filled with a packing 12 for distillation.

前記外筒体2は前記塔本体1の下端近くに位置させて縮径して形成した縮径部21と、この縮径部21の下端から垂直に延設した両端開口のジョイント用栓体22(オスジョイント)とを備える。空隙部20の下端及び塔本体1の開口下端部は縮径部を介して前記栓体22内と連通させてある。
前記外筒体2の上端はジョイント口管10の下端近くに位置させて塔本体1の上端部外周面に気密性を保持して溶着され、これより、空隙部20の上端は気密に閉塞されている。
The outer cylinder 2 is located near the lower end of the tower body 1 and has a reduced diameter portion 21 formed by reducing the diameter, and a joint plug 22 having both ends opened vertically extending from the lower end of the reduced diameter portion 21. (Male joint). The lower end of the gap portion 20 and the lower end portion of the opening of the tower body 1 are communicated with the inside of the plug body 22 through a reduced diameter portion.
The upper end of the outer cylinder 2 is positioned near the lower end of the joint port tube 10 and is welded to the outer peripheral surface of the upper end of the tower body 1 while maintaining airtightness. ing.

実施形態1の蒸留塔100は、図2に示すように、ジョイント用栓体22を蒸留釜3のジョイント口管30(メスジョイント)に気密に嵌挿して使用される。そして、蒸留釜3を加熱することにより、釜3内の液体混合物31から発生する蒸発蒸気は、栓体22内を通過して上昇し、同図矢印32で示すように塔本体1内に導入され、塔本体1内を上昇する。同時に前記蒸発蒸気は図2の矢印33で示すように分流して空隙部20内へ導入され、空隙部20内を上昇する。これにより、空隙部20内へ導入される前記蒸気により、前記空隙部に、塔本体1を与熱保温(加熱保温)する自己与熱保温効果を具備させるように構成してある。 As shown in FIG. 2, the distillation column 100 of the first embodiment is used by fitting the joint plug 22 into the joint port 30 (female joint) of the distillation still 3 in an airtight manner. Then, by heating the distillation kettle 3, the evaporated vapor generated from the liquid mixture 31 in the kettle 3 rises through the plug 22 and is introduced into the tower body 1 as indicated by an arrow 32 in the figure. And rises in the tower body 1. At the same time, the vaporized vapor is diverted as shown by an arrow 33 in FIG. Thereby, the vapor | steam introduce | transduced in the space | gap part 20 is comprised so that the said space | gap part may be provided with the self-heating heat retention effect which heat-heat-retains the column main body 1 (heating heat retention).

なお、図2において、34はモノヒート(マントルヒーター)、35はサンプル抜出し口、36はサンプル抜出し用注射器、37は温度調節器を示す。   In FIG. 2, 34 is a monoheat (mantle heater), 35 is a sample extraction port, 36 is a sample extraction syringe, and 37 is a temperature controller.

実施形態1の蒸留塔100は上記のように構成され、所望の器具を組み合わせて蒸留装置を構成して使用される。図3には実施形態1の蒸留塔を用いて構成した実験用の蒸留装置4の一例が開示されている。同図において、40は温度計、41は分留ヘッド、42及び43は冷却器、44はボールジョイント用クリップ、45は受留受器、46は丸底フラスコ、47は蒸留釜3に設けたキャピラリー栓、48は温度計を示す。   The distillation column 100 of Embodiment 1 is configured as described above, and is used by configuring a distillation apparatus by combining desired apparatuses. FIG. 3 discloses an example of an experimental distillation apparatus 4 configured using the distillation column of the first embodiment. In the figure, 40 is a thermometer, 41 is a fractionation head, 42 and 43 are coolers, 44 is a clip for a ball joint, 45 is a receiver, 46 is a round bottom flask, and 47 is provided in the still 3. Capillary stopper 48 is a thermometer.

次に実施形態1の蒸留塔を用いて実施した実験例の一例について説明する。図4は実施形態1の蒸留塔を用いて構成した理論段数測定用の蒸留装置5を示す。なお、図1及び図2において既に説明した構成と共通する構成等には同一符号を付して説明を省略する。   Next, an example of an experiment performed using the distillation column of Embodiment 1 will be described. FIG. 4 shows a distillation apparatus 5 for measuring the number of theoretical plates constructed using the distillation column of the first embodiment. In addition, the same code | symbol is attached | subjected to the structure etc. which are common in the structure already demonstrated in FIG.1 and FIG.2, and description is abbreviate | omitted.

図4において、50は冷却器、51はサンプル抜出し用のマイクロシリンジ、52は温度計、53はサンプル抜出し口兼用の蒸留釜内圧力測定用取出し口、54はサンプル抜出し用注射器、55は差圧計、56は同圧用コック、57,57は液の入出用ゴム栓、58,59は接続管を示す。また、図4において、冷却器50の上端は大気中に開放されている。   In FIG. 4, 50 is a cooler, 51 is a micro-syringe for sample extraction, 52 is a thermometer, 53 is an extraction port for measuring the pressure in the still used as a sample extraction port, 54 is a syringe for sample extraction, and 55 is a differential pressure gauge. , 56 are cocks for the same pressure, 57 and 57 are rubber stoppers for entering and exiting the liquid, and 58 and 59 are connection pipes. Moreover, in FIG. 4, the upper end of the cooler 50 is open | released in air | atmosphere.

実験例は、測定用試薬として、n‐ヘプタン(℃)及びメチルシクロヘキサン(℃)を約1対1(重量%)の割合で混合した液体混合物を用いた。
理論段数の測定は次のような方法で行なった。所定の電圧を印加し、充分時間を置いて還流が安定したところで、塔頂及び塔底(蒸留釜内)から液をサンプリングし、ガスクロ測定装置を使用して、組成分析を行なった。
In the experimental example, a liquid mixture in which n-heptane (° C.) and methylcyclohexane (° C.) were mixed at a ratio of about 1: 1 (% by weight) was used as a measuring reagent.
The number of theoretical plates was measured by the following method. When a predetermined voltage was applied and the reflux was stabilized after a sufficient time, the liquid was sampled from the top and bottom (in the distillation kettle), and composition analysis was performed using a gas chromatograph.

常法に従って、下記のフェンスケの式(数1)によって、蒸留塔の理論段数を算出した。   According to the usual method, the theoretical plate number of the distillation column was calculated by the following Fengke equation (Equation 1).

Figure 0005941380
Figure 0005941380

上記数1の式中、Nは理論段数、XDLは塔頂のn‐ヘプタン組成、XDHは塔頂のメチルシクロヘキサン組成、XWLは塔底のn‐ヘプタン組成、XWHは塔底のメチルシクロヘキサン組成を示す。
また、αはn‐ヘプタンとメチルシクロヘキサンの相対揮発度(常温では1.075を採用)を示す。
In the above formula 1, N is the number of theoretical plates, XDL is the n-heptane composition at the top of the tower, XDH is the methylcyclohexane composition at the top, XWL is the n-heptane composition at the bottom, and XWH is the methylcyclohexane composition at the bottom. Show.
Α represents the relative volatility of n-heptane and methylcyclohexane (1.075 is adopted at room temperature).

なお、充填物の量は、所定の充填密度(g/cc)となるように予め計算しておき、充填ムラができないように注意して充填することが肝要である。
また、蒸留塔の圧力損失は、図4に示すようなガラス製差圧計を作成し、蒸留水を入れて塔頂、塔底の水圧mmHOを実測した。
It is important that the amount of the filler is calculated in advance so as to have a predetermined filling density (g / cc), and is filled with care so as not to cause uneven filling.
Moreover, the pressure loss of the distillation column was measured by preparing a glass differential pressure gauge as shown in FIG. 4 and adding distilled water to measure the water pressure mmH 2 O at the top and bottom of the column.

本実験例では、蒸留塔として、蒸留塔本体内径25mm、充填高さ1500mm、外筒体外径60mm、高さ1550mmからなる図1に示す蒸留塔の塔本体に充填物452gを充填して構成した蒸留塔を用いた。前記充填物として、特開2011−125841号公報に記載の充填物を採用した。充填密度は0.614g/ccであった。   In this experimental example, the distillation column was constituted by filling the column main body of the distillation column shown in FIG. 1, which has an inner diameter of 25 mm, a packing height of 1500 mm, an outer cylinder outer diameter of 60 mm, and a height of 1550 mm, with a packing of 452 g. A distillation column was used. As the filler, a filler described in JP 2011-125841 A was employed. The packing density was 0.614 g / cc.

1Lの蒸留釜に蒸留塔とサンプル抜出し口兼用の蒸留釜内圧力測定用取出し口を取付け、n‐ヘプタンとメチルシクロヘキサンを各350g仕込み、マントルヒーター(100V、350W)を使用して加熱還流を行なった。全還流状態で還流を継続し、時々、塔頂からサンプルを抜出し、ガスクロ測定装置で組成分析を行なった。組成が安定したところで、蒸留釜から塔底サンプルを抜出し、フェンスケの式から理論段数を算出した。その算出結果を表1に示す。   Attach a distillation column and an outlet for measuring the pressure in the distillation kettle as a sample outlet to a 1 L distillation kettle, charge 350 g each of n-heptane and methylcyclohexane, and heat and reflux using a mantle heater (100 V, 350 W) It was. Refluxing was continued in the total reflux state, and a sample was sometimes withdrawn from the top of the column and composition analysis was performed with a gas chromatograph. When the composition was stable, the bottom sample was extracted from the distillation kettle, and the number of theoretical plates was calculated from the Fengke equation. The calculation results are shown in Table 1.

Figure 0005941380
Figure 0005941380

上記表1に示すように、電圧範囲80〜90Vで、理論段数58〜64段の性能が得られた。そのときの塔頂と蒸留釜の差圧は40〜90mmHOであった。なお、上記表1中、H.E.T.Pは1理論段当りの充填高さを示す。 As shown in Table 1 above, performance of 58 to 64 theoretical plates was obtained in the voltage range of 80 to 90V. At that time, the pressure difference between the top of the column and the distillation kettle was 40 to 90 mmH 2 O. In Table 1 above, H.M. E. T. T. et al. P indicates the filling height per theoretical plate.

図5は本発明の他の実施形態(実施形態2)を示す。この実施形態2及び以下に開示する各実施形態の蒸留塔において、実施形態1で既に説明した構成と共通する構成部等には同一符号を付して説明を省略する。   FIG. 5 shows another embodiment (Embodiment 2) of the present invention. In the distillation tower of the second embodiment and each embodiment disclosed below, the same reference numerals are given to the same components as those already described in the first embodiment, and the description thereof will be omitted.

実施形態2の蒸留塔200は、蒸留塔本体1Aの下端部を保温用の外筒体2の縮径部21の上端部に連通させると共に気密性を保持して外筒体2に溶着13して固定してある。また、実施形態2では、塔本体1Aの下端部に前記空隙部20と連通させて形成した任意数(図示では4個)の連通孔14,14が設けてある。   In the distillation column 200 of the second embodiment, the lower end portion of the distillation column main body 1A is communicated with the upper end portion of the reduced diameter portion 21 of the heat insulating outer cylindrical body 2 and is hermetically sealed and welded 13 to the outer cylindrical body 2. Fixed. In the second embodiment, an arbitrary number (four in the drawing) of communication holes 14 and 14 formed to communicate with the gap 20 are provided at the lower end of the tower main body 1A.

上記構成により、蒸留釜3内の液体混合物31から発生する蒸発蒸気は塔本体1内に導入され、図5に矢印aで示すように、塔本体1内を上昇する。また、塔本体1内に導入される前記蒸気の一部は、図5に矢印bで示すように、塔本体1内で分流して前記各孔14を通じて空隙部20内へ導入され、空隙部20内を上昇するように構成されている。これにより、空隙部20内へ導入される前記蒸気により、実施形態1と同様に、外筒体2に対し、塔本体1を与熱保(加熱保温)する自己与熱保温効果を具備させるように構成してある。他の構成は実施形態1と同様である。 With the above configuration, the evaporated vapor generated from the liquid mixture 31 in the distillation still 3 is introduced into the tower body 1 and ascends in the tower body 1 as indicated by an arrow a in FIG. Further, as shown by an arrow b in FIG. 5, a part of the steam introduced into the tower body 1 is divided in the tower body 1 and introduced into the cavity 20 through the holes 14. 20 is configured to rise. Thus, by the steam introduced into the gap portion 20, similarly to Embodiment 1, with respect to the outer cylinder 2, is provided with a self Azukanetsu heating effect of the column body 1 for Azukanetsuho temperature (heat insulation) It is constituted as follows. Other configurations are the same as those of the first embodiment.

実施形態2の蒸留塔は上記のように構成され、実施形態1と同様に使用するものであり、実施形態1と同様の作用効果を奏する。   The distillation column of the second embodiment is configured as described above and is used in the same manner as in the first embodiment, and has the same effects as those in the first embodiment.

図6は本発明のさらに他の実施形態(実施形態3)を示す。実施形態3の蒸留塔300は、実施形態1の蒸留塔100において、前記外筒体2のさらに外側に保温用真空ジャケット6を設けたことを特徴とするものである。他の構成は実施形態1と同様である。   FIG. 6 shows still another embodiment (Embodiment 3) of the present invention. The distillation column 300 of Embodiment 3 is the same as the distillation column 100 of Embodiment 1, except that a heat insulation vacuum jacket 6 is provided on the outer side of the outer cylinder 2. Other configurations are the same as those of the first embodiment.

実施形態3の蒸留塔は上記のように構成され、実施形態1と同様に使用するものであり、実施形態1の作用効果に加え、外筒体を保温する効果を奏する。実施形態3の蒸留塔は、例えば冬期の寒冷地等での実施に最適である。なお、この場合において、前記ジャケット6に代え、外筒体2の外周に断熱性の布地を被覆し、或いは発泡材等で外筒体2に断熱効果を具備させる構成、その他の保温手段を採用してもよい。   The distillation column of the third embodiment is configured as described above, and is used in the same manner as in the first embodiment. In addition to the effects of the first embodiment, there is an effect of keeping the outer cylinder warm. The distillation tower of Embodiment 3 is optimal for implementation in cold regions in winter, for example. In this case, instead of the jacket 6, a configuration in which the outer cylinder 2 is covered with a heat-insulating fabric, or the outer cylinder 2 is provided with a heat-insulating effect with a foam material or the like, or other heat retaining means is employed. May be.

なお、実施形態3においては、実施形態1の蒸留塔100の前記外筒体2の外側に保温用真空ジャケット6その他の保温手段を設ける例を開示したが、前記構成は実施形態2の蒸留塔200においても採用可能なこと勿論である。また、後述する各実施形態の蒸留塔にも採用することができる。   In the third embodiment, the example in which the heat insulation vacuum jacket 6 and other heat retaining means are provided outside the outer cylindrical body 2 of the distillation column 100 of the first embodiment has been disclosed. However, the configuration is the distillation tower of the second embodiment. Of course, it can also be adopted in 200. Moreover, it is employable also in the distillation tower of each embodiment mentioned later.

図7は本発明のさらに他の実施形態(実施形態4)を示す。実施形態4の蒸留塔400は、実施形態1の蒸留塔において、蒸気導出管部と冷却器とを設けた構成に特徴がある。   FIG. 7 shows still another embodiment (Embodiment 4) of the present invention. The distillation column 400 of the fourth embodiment is characterized in that the vapor outlet pipe portion and the cooler are provided in the distillation column of the first embodiment.

実施形態4の蒸留塔400は、前記空隙部20の上端部と連通させて前記外筒体2の上端部から上方部側へ向けて突出させて設けた蒸気導出管部7と、この導出管部7に装着して設けた冷却器8とを備える。   The distillation column 400 of the fourth embodiment includes a steam outlet pipe portion 7 provided to communicate with the upper end portion of the gap portion 20 and project from the upper end portion of the outer cylindrical body 2 toward the upper side, and the outlet pipe. And a cooler 8 mounted on the unit 7.

実施形態4の導出管部7は、所望の曲率で上方へ弯曲した弯曲管部70と、弯曲管部70から略垂直に延設した垂直管部71と、この垂直管部71の上端から略垂直に延設したジョイント口管72(メスジョイント)とを備える。   The outlet tube portion 7 of the fourth embodiment includes a bent tube portion 70 bent upward with a desired curvature, a vertical tube portion 71 extending substantially vertically from the bent tube portion 70, and substantially from the upper end of the vertical tube portion 71. And a joint mouth pipe 72 (female joint) extending vertically.

冷却器8は、導出管部7から導出される蒸発蒸気を冷却して液化(凝縮)する凝縮用の冷却器である。実施形態4の冷却器8は、所望の径及び長さの円筒状に形成した冷却室80と、冷却室80内に配置して設けた熱交換用(冷却用)のコイル管81(パイプ製コイル)と、冷却室80の一端部(図において下端部)を縮径して形成した縮径部82の先端(図において下端)から垂直に延設した両端開口のジョイント栓体83(オスジョイント)とを備える。前記栓体83は前記ジョイント口管72に気密に適合して嵌挿するように構成されている。   The cooler 8 is a condensing cooler that cools and vaporizes (condenses) the evaporated vapor led out from the lead-out pipe section 7. The cooler 8 according to the fourth embodiment includes a cooling chamber 80 formed in a cylindrical shape having a desired diameter and length, and a coil tube 81 for heat exchange (for cooling) provided in the cooling chamber 80 (made of pipe). Coil) and joint plug body 83 (male joint) having both ends opened vertically extending from the tip (lower end in the figure) of the reduced diameter part 82 formed by reducing one end part (lower end in the figure) of the cooling chamber 80. ). The plug 83 is configured to fit and fit into the joint port tube 72 in an airtight manner.

前記冷却室80は、所望の部位に所望の大きさの気体出口部84(圧力出口部)を備える。実施形態4の気体出口部84は、冷却室80の他端部(図において上端部)を縮径し、この縮径部の中央部から上方へ突出させて設けてある。前記出口部84の開口先端は大気中に開放されている。前記出口部84は息抜き用である。   The cooling chamber 80 includes a gas outlet portion 84 (pressure outlet portion) having a desired size at a desired portion. The gas outlet portion 84 of the fourth embodiment is provided by reducing the diameter of the other end portion (upper end portion in the drawing) of the cooling chamber 80 and projecting upward from the central portion of the reduced diameter portion. The opening tip of the outlet portion 84 is open to the atmosphere. The outlet 84 is for breathing.

前記コイル管81の両端部は気密性を保持して冷却室80外に突出させ、一端部で熱交換用流体(冷媒)の入口部85が、また、他端部で出口部86が形成されている。冷媒は入口部85から供給され、コイル管81を循環させて出口部86から流出させる。冷媒としては、例えば水道水,地下水,冷水等の液体が採用される。他の構成は実施形態1と同様である。   Both ends of the coil tube 81 are kept airtight and protrude out of the cooling chamber 80, and an inlet 85 for heat exchange fluid (refrigerant) is formed at one end, and an outlet 86 is formed at the other end. ing. The refrigerant is supplied from the inlet portion 85, circulates through the coil tube 81, and flows out from the outlet portion 86. As the refrigerant, for example, a liquid such as tap water, ground water, cold water or the like is employed. Other configurations are the same as those of the first embodiment.

実施形態4の蒸留塔400は上記のように構成され、冷却器8を蒸気導出管部7の上端部に装着して使用する以外は実施形態1と同様に使用される。   The distillation column 400 of the fourth embodiment is configured as described above, and is used in the same manner as in the first embodiment except that the cooler 8 is attached to the upper end portion of the vapor outlet pipe portion 7 and used.

実施形態4のように構成すると、空隙部20へ導入されて上昇する前記蒸発蒸気の一部は、図7(a)の矢印73で示すように、空隙部20の上端部から導出管部7へ導出し、導出管部7を通過して図7(b)の矢印74で示すように冷却器8の冷却室80内へ導入される。したがって、前記蒸気が上昇し易くなる。   When configured as in Embodiment 4, a part of the evaporating vapor that is introduced into the gap 20 and rises, as indicated by an arrow 73 in FIG. And is introduced into the cooling chamber 80 of the cooler 8 as shown by an arrow 74 in FIG. Therefore, the steam is likely to rise.

冷却室80内へ導入された前記蒸気は冷却室80内で冷却されて液化(凝縮)され、図7の矢印75で示すように流下し、導出管部7を通って空隙部20へ還流する。このように、実施形態4によれば、実施形態1の作用効果に加え、空隙部20へ導入された前記蒸気は、実施形態1と比べて上昇し易くなる。   The steam introduced into the cooling chamber 80 is cooled and liquefied (condensed) in the cooling chamber 80, flows down as indicated by an arrow 75 in FIG. 7, and returns to the gap portion 20 through the outlet pipe portion 7. . As described above, according to the fourth embodiment, in addition to the effects of the first embodiment, the steam introduced into the gap 20 is likely to rise as compared with the first embodiment.

なお、前記蒸気の導入により冷却室80内の圧力は高くなるが、冷却室80は気体出口部84を備えているので、所定値以上の圧力は前記出口部84から室外へ順次排出される。したがって、前記蒸気は室内へ連続的に安定して円滑に導入する。
また、冷却室80内へ導入される前記蒸気は冷却されて液化して流下するので、前記蒸気が前記出口部から排出することは無い。
Although the pressure in the cooling chamber 80 increases due to the introduction of the steam, the cooling chamber 80 includes the gas outlet portion 84, so that a pressure equal to or higher than a predetermined value is sequentially discharged from the outlet portion 84 to the outside of the room. Therefore, the steam is continuously and smoothly introduced into the room.
Further, since the steam introduced into the cooling chamber 80 is cooled and liquefied and flows down, the steam is not discharged from the outlet portion.

実施形態4の構成を具備した蒸留塔は、例えば、特に大型の蒸留塔に最適である。但し、小型の蒸留塔としても効果的に採用できること勿論である。   The distillation column provided with the configuration of Embodiment 4 is most suitable for a particularly large distillation column, for example. However, it is needless to say that it can be effectively employed as a small distillation column.

図8は本発明のさらに他の実施形態(実施形態5)を示す。実施形態5の蒸留塔500は、実施形態4の蒸留塔において、還流用管路を設けた構成に特徴がある。なお、実施形態5の蒸留塔において、実施形態4で既に説明した構成と共通する構成部等には同一符号を付して説明を省略する。   FIG. 8 shows still another embodiment (Embodiment 5) of the present invention. The distillation column 500 of Embodiment 5 is characterized in that the reflux column is provided in the distillation column of Embodiment 4. Note that in the distillation column of the fifth embodiment, the same reference numerals are given to the same components as those already described in the fourth embodiment, and the description thereof is omitted.

実施形態5の蒸留塔500は、実施形態4の蒸留塔において、一端部の先端を導出管部7と連通させて導出管部7に溶着その他の手段で気密性を保持して固定(実施形態5では溶着)すると共に他端部の先端を空隙部20と連通させて外筒部の所望の部位に溶着その他の手段で気密性を保持して固定(実施形態5では溶着)して設けた還流用管路9を備える。   The distillation column 500 of Embodiment 5 is the same as the distillation column of Embodiment 4 except that one end of the distillation column 500 communicates with the outlet tube portion 7 and is fixed to the outlet tube portion 7 with airtightness by welding or other means (Embodiment Mode). 5 is welded), and the tip of the other end portion is communicated with the gap portion 20 so as to be fixed to a desired portion of the outer cylinder portion by welding or other means (welding in the fifth embodiment). A reflux line 9 is provided.

還流用管路9は、前記他端部(図において下端部)にU字状管部90を備える。また、前記管路9には、一端部(図において上端部)の近くに位置させて管路9に介装して設けた開閉バルブ91を備える。実施形態5では、前記管路9の他端部(下端部)の先端を外筒体2の下端部近くに溶接して固定してある。前記U字状管部は、空隙部から管路9へ前記蒸気が導入するのを防止するために設けたものである。   The reflux conduit 9 includes a U-shaped tube 90 at the other end (the lower end in the figure). Further, the conduit 9 is provided with an open / close valve 91 provided near the one end (upper end in the drawing) and provided in the conduit 9. In the fifth embodiment, the distal end of the other end (lower end) of the conduit 9 is welded and fixed near the lower end of the outer cylinder 2. The U-shaped pipe part is provided to prevent the steam from being introduced from the gap part into the pipe line 9.

前記管路9は冷却器8の冷却室80内で液化した液体を流下させて空隙部20へ還流するもので、管の径は特に限定するものではないが、例えば、液体が流通可能な細径の管材を採用できる。前記バルブ91は、例えば、装置の稼動停止中や稼動開始当初、その他の所望ないし必要時に閉じるもので、それ以外は開いた状態にしておく。なお、このバルブ91は省略することも可能である。   The pipe 9 is used for allowing the liquid liquefied in the cooling chamber 80 of the cooler 8 to flow down and returning to the gap 20, and the diameter of the pipe is not particularly limited. Diameter pipe material can be used. The valve 91 is closed, for example, when the apparatus is not operating or at the beginning of the operation, when it is desired or necessary, and is otherwise open. The valve 91 can be omitted.

前記U字状管部90は空隙部20へ導入された前記蒸発蒸気が還流用管路9へ導入するのを防止するために設けたものである。他の構成は実施形態及び実施形態1と同様である。 The U-shaped tube portion 90 is provided to prevent the vaporized vapor introduced into the gap portion 20 from being introduced into the reflux conduit 9. Other configurations are the same as those in the fourth embodiment and the first embodiment.

実施形態5の蒸留塔500は上記のように構成され、実施形態と同様に冷却器8を蒸気導出管部7の上端部に装着して使用する以外は実施形態1と同様に使用される。 The distillation column 500 of the fifth embodiment is configured as described above, and is used in the same manner as in the first embodiment except that the cooler 8 is mounted on the upper end of the vapor outlet pipe portion 7 and used as in the fourth embodiment. .

実施形態5のように構成すると、冷却室80で液化した液体の大部分は、図8(a)の矢印92で示すように管路9を通って空隙部20の下端部側へ還流する。そのため、空隙部20を上昇する前記蒸気との接触が実施形態4と比べて少なくなる。したがって、還流する液体との接触による影響が実施形態4に比べて減少する。   When configured as in the fifth embodiment, most of the liquid liquefied in the cooling chamber 80 flows back to the lower end side of the gap 20 through the conduit 9 as indicated by an arrow 92 in FIG. Therefore, the contact with the vapor that rises in the gap 20 is less than that in the fourth embodiment. Therefore, the influence of the contact with the refluxing liquid is reduced as compared with the fourth embodiment.

実施形態5の構成を具備した蒸留塔は、実施形態4と同様に、例えば、特に大型の蒸留塔に最適である。但し、小型の蒸留塔としても効果的に採用できる。   The distillation column having the configuration of the fifth embodiment is optimal for a large distillation column, for example, as in the fourth embodiment. However, it can be effectively employed as a small distillation column.

なお、実施形態4及び実施形態5では、実施形態1の蒸留塔に前記構成を具備した例を開示したが、上記構成は実施形態2及び3の蒸留塔においても採用可能なこと勿論である。   In the fourth and fifth embodiments, the example in which the above-described configuration is provided in the distillation column of the first embodiment has been disclosed. However, it is needless to say that the above configuration can also be adopted in the distillation columns of the second and third embodiments.

また、上記した各実施形態では、充填塔で構成した蒸留塔を開示したが、充填等に代え、オルダーショウ塔、シープ塔、棚段塔、その他の任意の種類や形式の実験用及び工業用の蒸留塔を採用できること勿論である。   Further, in each of the above-described embodiments, a distillation column composed of a packed column is disclosed, but instead of packing or the like, Oldershaw Tower, Sheep Tower, Plate Tower, and any other types and types of experimental and industrial use are disclosed. Of course, a distillation column can be employed.

なお、上記した各実施形態の蒸留塔は一例として開示したもので、本発明は上記の実施形態に限定されるものではなく、特許請求の範囲に記載の技術思想を越脱しない範囲内において任意に変更可能なものである。   The distillation column of each of the above embodiments is disclosed as an example, and the present invention is not limited to the above embodiment, and may be arbitrarily selected without departing from the technical idea described in the claims. It can be changed to

1 蒸留塔本体
2 保温用の外筒体
3 蒸留釜
20 空隙部
31 液体混合物
DESCRIPTION OF SYMBOLS 1 Distillation tower main body 2 Outer cylinder 3 for heat insulation Distilling pot 20 Cavity 31 Liquid mixture

Claims (5)

蒸留塔において、
蒸留塔本体と、前記塔本体の外周面の略全域との間に略円筒状の空隙部を形成して設けた保温用の外筒体とを備え、
蒸留釜内の液体混合物から発生する蒸発蒸気を前記塔本体及び前記空隙部へ導入し、前記空隙部へ導入する前記蒸気により、前記空隙部に、前記塔本体を熱保温する自己与熱保温効果を具備させるように構成した
ことを特徴とする蒸留塔。
In the distillation tower,
A distillation column main body, and an outer cylinder for heat insulation provided by forming a substantially cylindrical void between the entire outer peripheral surface of the column main body,
Evaporation vapor generated from the liquid mixture of the distillation still was introduced into the tower body and the gap portion, by the steam introduced into the gap portion, the gap portion, a self Azukanetsu incubated for pressurizing the heat insulation of the tower body A distillation column characterized by having an effect.
請求項1に記載の蒸留塔において、前記外筒体の外側に保温用真空ジャケットその他の保温手段を設けたことを特徴とする蒸留塔。   2. The distillation column according to claim 1, wherein a heat insulation vacuum jacket and other heat insulation means are provided outside the outer cylindrical body. 前記空隙部と連通させて前記外筒体の上端部から上方部側へ向けて突出させて設けた蒸気導出管部と、
前記導出管部と連通させて前記導出管部の上端部に設けた冷却器とを備えている
ことを特徴とする請求項1に記載の蒸留塔。
A steam outlet pipe portion provided in communication with the gap and projecting upward from the upper end of the outer cylinder;
The distillation column according to claim 1, further comprising a cooler provided in communication with the outlet pipe portion and provided at an upper end portion of the outlet pipe portion.
前記空隙部と連通させて前記外筒部の上端部から上方部側へ向けて突出させて設けた蒸気導出管部と、
前記導出管部と連通させて前記導出管部の上端部に設けた冷却器と、
一端部の先端を前記導出管部と連通させて前記導出管部に気密性を保持して固定すると共に他端部の先端を前記空隙部と連通させて前記外筒体の所望の部位に気密性を保持して固定して設けた還流用管路とを備えている
ことを特徴とする請求項1に記載の蒸留塔。
A steam outlet pipe portion provided in communication with the gap and projecting upward from the upper end of the outer cylinder portion;
A cooler provided at the upper end of the outlet pipe portion in communication with the outlet pipe portion;
The tip of one end is communicated with the lead-out tube and is fixed to the lead-out tube while maintaining airtightness, and the tip of the other end is communicated with the gap and airtight to a desired part of the outer cylinder. The distillation column according to claim 1, further comprising a reflux conduit that is fixed while maintaining the property.
請求項4に記載の蒸留塔において、前記還流用管路は、前記他端部にU字状管部を備えていることを特徴とする蒸留塔。   The distillation column according to claim 4, wherein the reflux conduit includes a U-shaped tube portion at the other end.
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