JP2009101334A - Distilling apparatus of waste solvent containing solid component - Google Patents

Distilling apparatus of waste solvent containing solid component Download PDF

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JP2009101334A
JP2009101334A JP2007278260A JP2007278260A JP2009101334A JP 2009101334 A JP2009101334 A JP 2009101334A JP 2007278260 A JP2007278260 A JP 2007278260A JP 2007278260 A JP2007278260 A JP 2007278260A JP 2009101334 A JP2009101334 A JP 2009101334A
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waste solvent
evaporator
solvent
line
distillation
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Motoki Fujimoto
基 藤本
Masanori Torii
正憲 鳥井
Tsutomu Matoba
勉 的場
Takahisa Orii
孝久 折井
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HORIKAWA KASEI KK
NIPPON KAGAKU KIKAI SEIZO
Japan Chemical Engineering and Machinery Co Ltd
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HORIKAWA KASEI KK
NIPPON KAGAKU KIKAI SEIZO
Japan Chemical Engineering and Machinery Co Ltd
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a distilling apparatus capable of recovering solvent from waste solvent containing solid components with a high recovery rate, and removing the solid components remaining in the apparatus without stopping heating operation in an evaporator. <P>SOLUTION: The distilling apparatus is provided with the evaporator 10 heating and evaporating waste solvent containing solid components, a waste solvent drawing out line 14 discharging the waste solvent from the evaporator 10, a separation tank 20 receiving the waste solvent from the waste solvent drawing out line 14 for sedimentation of the waste solvent, and a supernatant line returning supernatant of the waste solvent subjected to the sedimentation in the separation tank 20 to the evaporator 10. Thus, the amount of the solvent discarded together with the solid components is reduced to recover the solvent with high recovery rate, without stopping the heating operation in the evaporator 10 when discharging the solid components. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

本発明は、固形成分を含有する廃溶剤を精製して有機溶剤を回収する蒸留装置に関する。   The present invention relates to a distillation apparatus for purifying a waste solvent containing a solid component and recovering an organic solvent.

電子部品等の洗浄工程では洗浄液として有機溶剤が広く使用されている。使用済みの有機溶剤(廃溶剤)は、従来より溶剤成分を回収し再利用することが行われており、その回収方法としては、廃溶剤を加熱して気化させ、気化した蒸気を凝縮させて回収する蒸留精製法が一般的である。   An organic solvent is widely used as a cleaning liquid in a cleaning process for electronic parts and the like. The used organic solvent (waste solvent) has been conventionally recovered and reused, and the recovery method is to heat and vaporize the waste solvent and condense the vaporized vapor. The distillation purification method to collect is common.

例えば、特許文献1には、不純物を含む溶剤を流下膜式リボイラ(蒸発器)で気化させ、気化した蒸気を精留部に送り、それを凝縮させて回収する蒸留装置が記載されている。
特開2001-9201号公報([0008],図1)
For example, Patent Document 1 describes a distillation apparatus that vaporizes a solvent containing impurities with a falling film type reboiler (evaporator), sends the vaporized vapor to a rectifying unit, and condenses and recovers it.
Japanese Patent Laid-Open No. 2001-9201 ([0008], FIG. 1)

従来の蒸留装置では、固形成分を含有する廃溶剤が蒸発器に間欠的又は連続的に供給されて加熱されると、廃溶剤中の揮発成分は気化して蒸留部に送られるが、固形成分は蒸発器に残留する。そのため、蒸発器の加熱運転を続けると、廃溶剤における固形成分の濃度が高くなり、固形成分の種類によっては廃溶剤の粘度が高くなって揮発成分の蒸発速度が低下することがある。また、固体成分の濃度が高いまま廃溶剤を加熱し続けると、加熱部の壁面に固体成分が固着して焦げ付くこともある。   In the conventional distillation apparatus, when the waste solvent containing solid components is intermittently or continuously supplied to the evaporator and heated, the volatile components in the waste solvent are vaporized and sent to the distillation section. Remains in the evaporator. For this reason, when the heating operation of the evaporator is continued, the concentration of the solid component in the waste solvent increases, and depending on the type of the solid component, the viscosity of the waste solvent increases and the evaporation rate of the volatile component may decrease. Further, if the waste solvent is continuously heated while the concentration of the solid component is high, the solid component may adhere to the wall surface of the heating unit and may be burnt.

これを防ぐためには、蒸発器内で廃溶剤中の固体成分の濃度が高くなり過ぎる前に、蒸発器から固形成分を取り除く必要がある。その際に従来の蒸留装置では、固形成分とともに蒸発器内に残存する溶剤も取り除かれるため、多くの溶剤が再利用されずに廃棄される。また、固形成分を取り除く際に蒸発器の加熱運転を停止すると、熱エネルギーや時間のロスが生じ、非効率である。   In order to prevent this, it is necessary to remove the solid component from the evaporator before the concentration of the solid component in the waste solvent becomes too high in the evaporator. At that time, in the conventional distillation apparatus, the solvent remaining in the evaporator is removed together with the solid components, so that a large amount of the solvent is discarded without being reused. Further, if the heating operation of the evaporator is stopped when removing the solid components, heat energy and time are lost, which is inefficient.

本発明が解決しようとする課題は、固形成分を含有する廃溶剤から高い回収率で溶剤を回収するとともに、蒸発器の加熱運転を停止することなく装置に残留する固形成分を取り除くことができる蒸留装置を提供することである。   The problem to be solved by the present invention is a distillation capable of recovering a solvent from a waste solvent containing a solid component at a high recovery rate and removing the solid component remaining in the apparatus without stopping the heating operation of the evaporator. Is to provide a device.

上記課題を解決するために成された本発明に係る蒸留装置は、
固形成分を含有する廃溶剤から溶剤成分を回収する蒸留装置において、
前記廃溶剤を加熱して溶剤成分を気化させる蒸発器と、
前記蒸発器から前記廃溶剤を流出させる廃溶剤ラインと、
前記廃溶剤ラインから前記廃溶剤を受け、該廃溶剤を沈降分離する分離槽と、
前記分離槽で沈降分離された廃溶剤の上澄液を前記蒸発器に戻す上澄液ラインと、
を備えることを特徴とする。
The distillation apparatus according to the present invention, which has been made to solve the above problems,
In a distillation apparatus that recovers a solvent component from a waste solvent containing a solid component,
An evaporator for heating the waste solvent to vaporize a solvent component;
A waste solvent line for draining the waste solvent from the evaporator;
A separation tank for receiving the waste solvent from the waste solvent line and settling and separating the waste solvent;
A supernatant line for returning the supernatant of the waste solvent settled and separated in the separation tank to the evaporator;
It is characterized by providing.

廃溶剤としては溶剤に固形成分が混入したものを対象とする。本発明に係る蒸留装置では、廃溶剤の溶剤成分は蒸発器内で蒸気となり廃溶剤から分離される。廃溶剤の固形成分は、まだ気化していない溶剤成分とともに蒸発器から分離槽に送られる。分離槽に送られた廃溶剤(固形成分及び溶剤成分)は分離槽にて沈降分離され、固形成分は沈殿し、溶剤成分は上澄液となる。沈殿した固形成分は分離槽から排出され、上澄液は上澄液ラインにより蒸発器に戻される。   The waste solvent is a solvent in which a solid component is mixed. In the distillation apparatus according to the present invention, the solvent component of the waste solvent becomes vapor in the evaporator and is separated from the waste solvent. The solid component of the waste solvent is sent from the evaporator to the separation tank together with the solvent component that has not been vaporized. The waste solvent (solid component and solvent component) sent to the separation tank is settled and separated in the separation tank, the solid component is precipitated, and the solvent component becomes a supernatant. The precipitated solid component is discharged from the separation tank, and the supernatant is returned to the evaporator by the supernatant line.

本発明に係る蒸留装置では、分離槽で分離された上澄液(溶剤成分)は分離槽から蒸発器に戻され、固形成分は分離槽から排出される。これにより、固形成分とともに溶剤成分が無駄に廃棄されることがなくなり、廃溶剤から高い回収率で溶剤を回収することができる。   In the distillation apparatus according to the present invention, the supernatant (solvent component) separated in the separation tank is returned from the separation tank to the evaporator, and the solid component is discharged from the separation tank. As a result, the solvent component is not wasted together with the solid component, and the solvent can be recovered from the waste solvent at a high recovery rate.

また、本発明に係る蒸留装置は、蒸発器とは別に設けた分離槽にて固形成分を沈殿させて排出するため、蒸発器の加熱運転を停止することなく装置に残留する固形成分を取り除くことができる。従って、熱エネルギーや時間のロスが生じず、効率よく蒸留を行うことができる。   Moreover, since the distillation apparatus according to the present invention precipitates and discharges solid components in a separation tank provided separately from the evaporator, the solid components remaining in the apparatus are removed without stopping the heating operation of the evaporator. Can do. Accordingly, heat energy and time are not lost, and distillation can be performed efficiently.

以下、添付図面に基づき、本発明の一実施例である蒸留装置を説明する。   Hereinafter, a distillation apparatus according to an embodiment of the present invention will be described with reference to the accompanying drawings.

図1は本実施例に係る蒸留装置の概略構成図である。この蒸留装置は、固形成分を含有する廃溶剤を加熱して気化させる蒸発缶10と、蒸発缶10の下方に設けられ蒸発缶10で濃縮された廃溶剤を沈降分離する分離槽20と、蒸発缶10より流入する廃溶剤蒸気を沸点の違いを利用して分離する蒸留塔40とを主な構成要素とする。   FIG. 1 is a schematic configuration diagram of a distillation apparatus according to the present embodiment. This distillation apparatus includes an evaporator 10 that heats and vaporizes a waste solvent containing a solid component, a separation tank 20 that is provided below the evaporator 10 and settles and separates the waste solvent concentrated by the evaporator 10, and evaporation A distillation column 40 that separates waste solvent vapor flowing in from the can 10 using a difference in boiling point is a main component.

蒸発缶10の上部には、蒸発缶10に廃溶剤を供給する廃溶剤供給ライン11を接続する。蒸発缶10の内部には、水蒸気の熱により蒸発缶10内の廃溶剤を間接加熱する加熱部12を設ける。加熱部12はメンテナンス等において洗浄しやすくするために蒸発缶10から取り外し可能にしておくことが望ましい。加熱部12に水蒸気を送る第1水蒸気供給ライン13は、加熱部12だけでなく蒸発缶10にも接続し、蒸発缶10の缶内にも水蒸気を供給可能にする。なお、廃溶剤供給ライン11、第1水蒸気供給ライン13及び以下に述べる各ラインは、その中を流れる流体の流量調整を行うバルブや流量測定を行う流量計等を適宜備える。   A waste solvent supply line 11 that supplies waste solvent to the evaporator 10 is connected to the upper part of the evaporator 10. Inside the evaporator 10, a heating unit 12 that indirectly heats the waste solvent in the evaporator 10 with the heat of water vapor is provided. The heating unit 12 is desirably removable from the evaporator 10 in order to facilitate cleaning during maintenance or the like. The first water vapor supply line 13 for sending water vapor to the heating unit 12 is connected not only to the heating unit 12 but also to the evaporator 10, and can supply water vapor into the can of the evaporator 10. The waste solvent supply line 11, the first water vapor supply line 13, and each line described below appropriately include a valve for adjusting the flow rate of the fluid flowing through the waste solvent supply line 11, a flow meter for measuring flow rate, and the like.

蒸発缶10の底部と分離槽20の上部とは廃溶剤抜き出しライン14で接続し、蒸発缶10内の廃溶剤を自然流下させて分離槽20に抜き出すようにする。廃溶剤抜き出しライン14中の蒸発缶10近傍には、廃溶剤の流量を調整する廃溶剤抜き出しバルブ15を設ける。廃溶剤抜き出しライン14中の廃溶剤抜き出しバルブ15よりも下流側(分離槽20側)には、圧縮空気を管内に送る圧縮空気供給ライン16を接続する。なお、廃溶剤抜き出しバルブ15をはじめ本実施例におけるバルブは電磁気もしくは空気圧によって開閉作動する自動弁とする。   The bottom of the evaporator 10 and the top of the separation tank 20 are connected by a waste solvent extraction line 14 so that the waste solvent in the evaporator 10 flows down naturally and is extracted into the separation tank 20. A waste solvent extraction valve 15 for adjusting the flow rate of the waste solvent is provided in the vicinity of the evaporator 10 in the waste solvent extraction line 14. A compressed air supply line 16 for sending compressed air into the pipe is connected to the downstream side of the waste solvent extraction valve 15 in the waste solvent extraction line 14 (on the separation tank 20 side). Note that the waste solvent extraction valve 15 and other valves in this embodiment are automatic valves that open and close by electromagnetic or pneumatic pressure.

分離槽20は筒状の壁面の下端に、下に凸の円錐状の底部が連結したものとし、壁面の上端は天板で閉じる。分離槽20の下方には、廃溶剤の沈降分離により生じるスラリーを溜めるドラム缶21を配置する。分離槽20の底部先端とドラム缶21の上面とを接続するスラリー抜き出しライン24には、スラリーの排出時期を制御するスラリー抜き出しバルブ35を設ける。スラリー抜き出しライン24とスラリー抜き出しバルブ35は固形成分による閉塞を防止するために150A以上の大口径のものにすることが望ましい。分離槽20の上方には分離槽20内で廃溶剤から発生する蒸気を凝縮させる廃溶液コンデンサ22を配置し、廃溶液コンデンサ22の入口及び出口は凝縮ライン23により分離槽20の上部に接続する。   The separation tank 20 is connected to the lower end of the cylindrical wall surface with a conical bottom that is convex downward, and the upper end of the wall surface is closed with a top plate. Below the separation tank 20, a drum can 21 is disposed for storing slurry generated by sedimentation and separation of the waste solvent. The slurry extraction line 24 that connects the bottom end of the separation tank 20 and the upper surface of the drum can 21 is provided with a slurry extraction valve 35 that controls the discharge timing of the slurry. It is desirable that the slurry extraction line 24 and the slurry extraction valve 35 have a large diameter of 150 A or more in order to prevent clogging by solid components. Above the separation tank 20 is disposed a waste solution capacitor 22 for condensing vapor generated from the waste solvent in the separation tank 20, and the inlet and outlet of the waste solution capacitor 22 are connected to the upper part of the separation tank 20 by a condensation line 23. .

分離槽20の壁面には、廃溶剤の上澄液の流出口である3本の上澄液流出口(第1上澄液流出口25、第2上澄液流出口26、第3上澄液流出口27)を異なる高さに設置する。各上澄液流出口は上澄液流出ライン28によって各上澄液流出口よりも低い位置に配置した一時貯留槽29に接続する。一時貯留槽29はポンプ31を備えた上澄液循環ライン30により蒸発缶10の上部と接続する。上澄液循環ライン30のポンプ31よりも下流側(蒸発缶10側)には廃液タンクに繋がる廃液ライン34を接続する。   On the wall surface of the separation tank 20, there are three supernatant outlets (first supernatant outlet 25, second supernatant outlet 26, and third supernatant, which are outlets for the supernatant of the waste solvent. The liquid outlets 27) are installed at different heights. Each supernatant outlet is connected to a temporary storage tank 29 disposed at a position lower than each supernatant outlet by a supernatant outlet line 28. The temporary storage tank 29 is connected to the upper part of the evaporator 10 by a supernatant circulation line 30 equipped with a pump 31. A waste liquid line 34 connected to a waste liquid tank is connected to a downstream side (evaporator 10 side) of the supernatant liquid circulation line 30 from the pump 31.

蒸発缶10における廃溶剤蒸気の出口には、蒸気に同伴するミストを捕集するワイヤーメッシュデミスタ33を設置する。なお、ワイヤーメッシュデミスタ33の代わりに干渉板や規則充填物等を用いてもよい。干渉板としては、折り曲げた板を並列させた、いわゆるコレクタを利用したもの、逆円錐状のもの、ラジエータ状のもの等を用いることができる。蒸発缶10における廃溶剤蒸気の出口は、蒸気ライン32により蒸留塔40の側面と接続する。   At the outlet of the waste solvent vapor in the evaporator 10, a wire mesh demister 33 that collects mist accompanying the vapor is installed. In place of the wire mesh demister 33, an interference plate, regular packing, or the like may be used. As the interference plate, a so-called collector using bent plates, an inverted cone, a radiator, or the like can be used. The outlet of the waste solvent vapor in the evaporator 10 is connected to the side surface of the distillation column 40 by the vapor line 32.

蒸留塔40は、その中に廃溶液蒸気を通過させることにより、廃溶液に含まれ沸点が異なる各成分を分離して凝縮させるものである。そのために、蒸留塔40内には、通過する蒸気と接触させるための4つの充填物(下から順に第1充填物41、第2充填物42、第3充填物43、第4充填物44)を設置する。各充填物では、それ自体のみならず、充填物で既に凝縮された液体と蒸気が接触することにより、蒸気の凝縮が促進される。各充填物には、液体の負荷変動や精密蒸留に対応可能な、規則的な構造を有する規則充填物を用いることが望ましい。なお、蒸発缶10の廃溶剤蒸気の出口は、蒸気ライン32により第1充填物41と第2充填物42の間の蒸留塔40側面に接続する。   The distillation tower 40 is configured to separate and condense components having different boiling points contained in the waste solution by passing the waste solution vapor therethrough. Therefore, in the distillation column 40, there are four packings (first packing 41, second packing 42, third packing 43, and fourth packing 44 in order from the bottom) for contacting with the passing steam. Is installed. For each packing, vapor condensation is facilitated by contact of the vapor with the liquid already condensed in the packing, as well as the packing itself. For each packing, it is desirable to use a regular packing having a regular structure that can cope with liquid load fluctuations and precision distillation. Note that the outlet of the waste solvent vapor of the evaporator 10 is connected to the side surface of the distillation tower 40 between the first packing 41 and the second packing 42 by the steam line 32.

各充填物の直上には、上方より供給される液体を下方の各充填物に分散供給する4台の液分散装置(下から順に第1液分散装置45、第2液分散装置46、第3液分散装置47、第4液分散装置48)を設置する。図2は蒸留塔40内に設置した第1液分散装置45の縦断面図である。第1液分散装置45は、上方より供給される液体を蒸留塔40の横断面の中心部に集めるコレクタ71を上部に有する。コレクタ71中央の下方にはコレクタ71により集められた液体を導入する内側筒部72を設置し、内側筒部72の外側には、内側筒部72との間に隙間を設けた外側筒部73を設置する。内側筒部72の下部は水平面内でフィッシュボーン形に枝分かれするパイプから成る下側分散管74と接続し、外側筒部73の下部も下側分散管74と同様の形状を有する上側分散管75と接続する。ここで、下側分散管74及び上側分散管75の平面図を図3に示す。下側分散管74は、図3(a)に示すようにフィッシュボーンの背骨にあたる中央パイプ77と、その両側に中央パイプ77と直交して水平に延伸する片側5本(両側10本)の分枝パイプ78とから成る。同様に上側分散管75は、図3(b)に示すようにフィッシュボーンの背骨にあたる中央パイプ79と、その両側に中央パイプ79と直交して水平に延伸する片側6本(両側12本)の分枝パイプ80とから成る。分枝パイプ78、80の底部には細孔76、81を適宜設ける。このとき、分枝パイプ80の細孔81は下方から見て下側分散管74と重ならない位置に配置する。なお、第1液分散装置45以外の液分散装置も同様の構成を有する。   Immediately above each packing, there are four liquid dispersing devices (the first liquid dispersing device 45, the second liquid dispersing device 46, the third liquid dispersing device in this order from the bottom). A liquid dispersion device 47 and a fourth liquid dispersion device 48) are installed. FIG. 2 is a longitudinal sectional view of the first liquid dispersion device 45 installed in the distillation column 40. The first liquid dispersion device 45 has a collector 71 at the top for collecting the liquid supplied from above at the center of the cross section of the distillation column 40. An inner cylindrical portion 72 for introducing the liquid collected by the collector 71 is installed below the center of the collector 71, and an outer cylindrical portion 73 provided with a gap between the inner cylindrical portion 72 and the outer cylindrical portion 72. Is installed. The lower part of the inner cylinder part 72 is connected to a lower dispersion pipe 74 made of a pipe that branches into a fishbone shape in a horizontal plane, and the lower part of the outer cylinder part 73 also has an upper dispersion pipe 75 having the same shape as the lower dispersion pipe 74. Connect with. Here, a plan view of the lower dispersion pipe 74 and the upper dispersion pipe 75 is shown in FIG. As shown in FIG. 3A, the lower dispersion pipe 74 is divided into a central pipe 77 corresponding to the backbone of the fishbone and five sides (10 on both sides) extending horizontally on the both sides at right angles to the central pipe 77. And branch pipe 78. Similarly, as shown in FIG. 3B, the upper dispersion pipe 75 includes a central pipe 79 corresponding to the backbone of the fishbone, and six pipes on one side (12 pipes on both sides) extending horizontally at right angles to the central pipe 79 on both sides. It consists of a branch pipe 80. The pores 76 and 81 are appropriately provided at the bottoms of the branch pipes 78 and 80. At this time, the pores 81 of the branch pipe 80 are arranged at positions that do not overlap the lower dispersion pipe 74 when viewed from below. Note that liquid dispersion devices other than the first liquid dispersion device 45 have the same configuration.

蒸留塔40の塔頂部には、塔頂部から留出する精製物を凝縮させて戻す還流ラインを設ける。この還流ラインは第1パイプ50、精製物コンデンサ49、第2パイプ51、第3パイプ52がこの順に連結したものとし、塔頂部からの精製物もこの順に流れる。第2パイプ51、第3パイプ52の各端部が連結する連結部66には精製物コンデンサ49で凝縮した精製物を外に抜き出すための抜き出しライン53を接続する。   A reflux line is provided at the top of the distillation column 40 to condense and return the purified product distilled from the top. In this reflux line, the first pipe 50, the purified product condenser 49, the second pipe 51, and the third pipe 52 are connected in this order, and the purified product from the top of the tower also flows in this order. An extraction line 53 for extracting the purified product condensed by the purified product condenser 49 is connected to a connecting portion 66 to which the respective ends of the second pipe 51 and the third pipe 52 are connected.

廃溶剤に含まれる微量の低沸点成分を除去して主成分である溶剤を回収するために、最上部の第4充填物44とその下方の第3充填物43の間、及び第3充填物43とその下方の第2充填物42の間における蒸留塔40の側面には第2サイドカット口55、及び第1サイドカット口54をそれぞれ設ける。各サイドカット口は回収ライン56に繋げる。回収ライン56には各サイドカット口より留出した溶剤を冷水で冷却する溶剤クーラー62を設ける。この回収ライン56は抜き出しライン53よりも内径が太いパイプを使用し、必要な処理量に対応可能にする。また、溶剤クーラー62よりも上流側(蒸留塔40側)の回収ライン56と還流ラインにおける連結部66とはバイパスライン58で接続する。   In order to remove a small amount of low-boiling components contained in the waste solvent and recover the solvent as the main component, the third filler is placed between the uppermost fourth filler 44 and the third filler 43 below it. A second side cut port 55 and a first side cut port 54 are respectively provided on the side surface of the distillation column 40 between 43 and the second packing 42 below. Each side cut port is connected to a collection line 56. The recovery line 56 is provided with a solvent cooler 62 that cools the solvent distilled from each side cut port with cold water. The collection line 56 uses a pipe having an inner diameter larger than that of the extraction line 53, and can cope with a necessary processing amount. Further, the recovery line 56 on the upstream side (distillation tower 40 side) of the solvent cooler 62 and the connecting portion 66 in the reflux line are connected by a bypass line 58.

蒸留塔40の底部は再加熱ライン63と接続し、再加熱ライン63には蒸留塔40の底部に溜まった液体を水蒸気の熱により間接加熱するリボイラ59を設ける。リボイラ59に水蒸気を送る第2水蒸気供給ライン60は、リボイラ59だけでなく蒸留塔40の底部にも接続し、蒸留塔40内にも水蒸気を供給可能にする。再加熱ライン63のうち蒸留塔40の底部からリボイラ59に向かう位置に、廃液タンクに繋がる排水ライン65を接続する。排水ライン65には排水ポンプ61を設ける。   The bottom of the distillation column 40 is connected to a reheating line 63, and the reheating line 63 is provided with a reboiler 59 that indirectly heats the liquid accumulated at the bottom of the distillation column 40 by the heat of steam. The second water vapor supply line 60 for sending water vapor to the reboiler 59 is connected not only to the reboiler 59 but also to the bottom of the distillation column 40 so that the water vapor can be supplied into the distillation column 40. A drain line 65 connected to the waste liquid tank is connected to the reheating line 63 at a position from the bottom of the distillation column 40 toward the reboiler 59. A drainage pump 61 is provided in the drainage line 65.

このような構成を有する本実施例に係る蒸留装置を用いて、固形成分を含む廃溶剤から溶剤を回収する例を説明する。なお、一般的に廃溶剤には水が混入するが、本実施例に係る蒸留装置では廃溶剤に水が混入していても構わない。まず、廃溶剤が廃溶剤供給ライン11から蒸発缶10に間欠的又は連続的に流入する。蒸発缶10に流入した廃溶剤は加熱部12により加熱され、溶剤成分の蒸発に伴って濃縮される。蒸発缶10内における廃溶剤の固形成分の濃度は5〜10%に保つことが望ましいが、固形成分が非粘着性のものである場合等では固形成分の濃度を20〜30%にしてもよい。なお、第1水蒸気供給ライン13から蒸発缶10内に水蒸気を直接供給すれば、蒸発缶10内の温度が素早く上昇するため、装置の立ち上がり時間を短縮することができる。また、メンテナンスの際に蒸発缶10内に水蒸気を直接供給すれば、蒸発缶10内を洗浄することもできる。   An example in which a solvent is recovered from a waste solvent containing a solid component using the distillation apparatus according to the present embodiment having such a configuration will be described. In general, water is mixed in the waste solvent, but in the distillation apparatus according to the present embodiment, water may be mixed in the waste solvent. First, the waste solvent flows intermittently or continuously from the waste solvent supply line 11 into the evaporator 10. The waste solvent that has flowed into the evaporator 10 is heated by the heating unit 12 and concentrated as the solvent component evaporates. It is desirable to maintain the concentration of the solid component of the waste solvent in the evaporator 10 at 5 to 10%. However, when the solid component is non-adhesive, the concentration of the solid component may be 20 to 30%. . In addition, if water vapor | steam is directly supplied in the evaporator 10 from the 1st water vapor | steam supply line 13, since the temperature in the evaporator 10 will rise quickly, the start-up time of an apparatus can be shortened. Moreover, if water vapor | steam is directly supplied in the evaporator 10 in the case of a maintenance, the inside of the evaporator 10 can also be wash | cleaned.

蒸発缶10で気化した廃溶剤の蒸気は、ワイヤーメッシュデミスタ33を通過して蒸留塔40に連続的に送られる。ワイヤーメッシュデミスタ33では、蒸気に同伴するミストが捕集されるため、固体成分を含むミストはここで阻止される。   The waste solvent vapor evaporated in the evaporator 10 passes through the wire mesh demister 33 and is continuously sent to the distillation tower 40. In the wire mesh demister 33, since the mist accompanying the vapor is collected, the mist containing the solid component is blocked here.

蒸留塔40に入った蒸気は第1〜第4充填物41〜44の内部を通過する際に各充填物及び各充填物に既に付着している液体と接触することにより、その一部が凝縮する。このとき、蒸発缶10からの蒸気やリボイラ59で気化した蒸気によって蒸留塔40内は低位置ほど高温になるため、蒸留塔40に入った蒸気のうち高沸点成分は低位置の充填物で凝縮し、低沸点成分は低位置の充填物では凝縮せずに通過して蒸留塔40のより上部にまで到達しやすい。   When the vapor entering the distillation column 40 passes through the insides of the first to fourth packings 41 to 44, a part of the steam is condensed by coming into contact with each packing and the liquid already attached to each packing. To do. At this time, since the inside of the distillation column 40 becomes hot at the lower position due to the vapor from the evaporator 10 or the vaporized by the reboiler 59, the high boiling point component of the vapor entering the distillation tower 40 is condensed by the low-position packing. However, the low boiling point component passes through without being condensed in the packing at the lower position and easily reaches the upper part of the distillation column 40.

蒸留塔40の塔頂部に到達した蒸気は第1パイプ50を通って精製物コンデンサ49に入り、精製物コンデンサ49内を流れる冷却水によって凝縮する。凝縮物の一部は第2パイプ51、第3パイプ52を経て蒸留塔40の上部に還流され、その他は回収される。廃溶剤中に回収溶剤よりも低沸点の成分が含まれる場合、精製物コンデンサ49で凝縮した凝縮物にはその低沸点成分が多く含まれるため、バイパスライン58のバルブを閉じて抜き出しライン53より凝縮物を抜き出す。このとき、回収溶剤は第一サイドカット口54、もしくは第二サイドカット口55を経由して回収ライン56より回収する。一方、廃溶剤中に回収溶剤よりも低沸点の成分が含まれていない場合には、バイパスライン58のバルブを開け、精製物コンデンサ49で凝縮した凝縮物を回収ライン56を経由して回収する。   The vapor that has reached the top of the distillation column 40 enters the purified product condenser 49 through the first pipe 50 and is condensed by the cooling water flowing in the purified product condenser 49. A part of the condensate is refluxed to the upper part of the distillation column 40 through the second pipe 51 and the third pipe 52, and the other is recovered. If the waste solvent contains a component having a boiling point lower than that of the recovered solvent, the condensed product condensed in the refined product condenser 49 contains a large amount of the low boiling component, so the valve of the bypass line 58 is closed and the extraction line 53 is closed. Extract the condensate. At this time, the recovered solvent is recovered from the recovery line 56 via the first side cut port 54 or the second side cut port 55. On the other hand, when the waste solvent does not contain a component having a boiling point lower than that of the recovery solvent, the valve of the bypass line 58 is opened and the condensate condensed by the purified product condenser 49 is recovered via the recovery line 56. .

最上部の第4充填物44では凝縮しやすいがその下方の第3充填物43では蒸気のまま通過しやすい精製物は、第2サイドカット口55から抜き出す。同様に、第3充填物43では凝縮しやすいがその下方の第2充填物42では蒸気のまま通過しやすいものは、第1サイドカット口54から抜き出す。その際、第1サイドカット口54及び第2サイドカット口55は一方のみを開いて精製物を抜き出す。このようにサイドカット口を複数設けることにより、サイドカット口の開閉を切り替えるだけで回収する精製物の種類を迅速に変更することができるため、廃溶剤の溶剤成分の割合が変動する場合などの操作性が向上する。なお、第1サイドカット口54及び第2サイドカット口55より抜き出された液は回収ライン56を流れ、溶剤クーラー62にて冷却されて回収される。   The purified product which is easy to condense in the uppermost fourth packing 44 but easily passes through the third packing 43 below is extracted from the second side cut port 55. Similarly, the third filling 43 that is likely to condense but the second filling 42 below it is likely to pass through as steam and is extracted from the first side cut port 54. At that time, only the first side cut port 54 and the second side cut port 55 are opened, and the purified product is extracted. By providing a plurality of side cut ports in this way, the type of purified product to be recovered can be quickly changed simply by switching the opening and closing of the side cut ports, such as when the ratio of the solvent component of the waste solvent varies Operability is improved. Note that the liquid extracted from the first side cut port 54 and the second side cut port 55 flows through the recovery line 56 and is cooled and recovered by the solvent cooler 62.

蒸留塔40内の各充填物で凝縮した液体は重力により下方に流れる。流下する液体はその量の多少に関わらず、第1〜第4液分散装置45〜48によって、下方にある各充填物の上面全体に分散して供給される。その様子を図2、3を用いて説明する。第2充填物42の下面から流下する液体はコレクタ71により中央に集められ、内側筒部72に導入される。導入された液体は内側筒部72の下部から下側分散管74の中央パイプ77に流れ、そこから分枝パイプ78に枝分かれする。枝分かれした液体は分枝パイプ78の底部に設けた細孔76から下方に流出する。第2充填物42の下面から供給される液体の量が多くなり、内側筒部72の上端の開口部から液体が溢れ出すと、溢れた液体は内側筒部72と外側筒部73の間の隙間に流入する。隙間に流入した液体は、下側分散管74と同様、外側筒部73の下部から上側分散管75の中央パイプ79に流れ、そこから分枝パイプ80に枝分かれし、分枝パイプ80の底部に設けた細孔81から下方に流出する。このとき、細孔81は下方から見て分枝パイプ78と重ならない位置に設けられているため、細孔76、81から流出する液体は第1充填物41の上面の異なる位置に流れ落ちる。このようにフィッシュボーン形の分散管を2段以上にすることにより、液体の操作範囲が広がり、液の負荷変動に対処しやすくなる。なお、一般的にフィッシュボーン形の分散管はオープンチャネル形の分散管と比べ、液保有量が少ないため、品種切替を迅速に行うことができる。   The liquid condensed in each packing in the distillation column 40 flows downward by gravity. Regardless of the amount of the liquid that flows down, the liquid is distributed and supplied to the entire upper surface of each filling material by the first to fourth liquid dispersing devices 45 to 48. This will be described with reference to FIGS. The liquid flowing down from the lower surface of the second filler 42 is collected in the center by the collector 71 and introduced into the inner cylindrical portion 72. The introduced liquid flows from the lower part of the inner cylindrical part 72 to the central pipe 77 of the lower dispersion pipe 74 and then branches to the branch pipe 78. The branched liquid flows downward from the pores 76 provided at the bottom of the branch pipe 78. When the amount of liquid supplied from the lower surface of the second filling 42 increases and the liquid overflows from the opening at the upper end of the inner cylindrical portion 72, the overflowed liquid is between the inner cylindrical portion 72 and the outer cylindrical portion 73. It flows into the gap. Like the lower dispersion pipe 74, the liquid flowing into the gap flows from the lower part of the outer cylindrical portion 73 to the central pipe 79 of the upper dispersion pipe 75, branches from there to the branch pipe 80, and reaches the bottom of the branch pipe 80. It flows out downward from the provided pores 81. At this time, since the pore 81 is provided at a position that does not overlap the branch pipe 78 when viewed from below, the liquid flowing out from the pores 76 and 81 flows down to a different position on the upper surface of the first filling 41. In this way, by providing two or more fishbone-shaped dispersion pipes, the liquid operating range is widened, and it becomes easy to cope with liquid load fluctuations. In general, the fishbone type dispersion pipe has a smaller liquid holding amount than the open channel type dispersion pipe, so that the product type can be switched quickly.

最も低い位置にある第1充填物41において凝縮する成分は水などの高沸点成分であり、これは蒸留塔40の底部に液体の状態で溜まる。溜まった液体はリボイラ59に送られ、そこで間接加熱されて蒸気となり、蒸留塔40の底部に戻って蒸留塔40内を上昇する。また、一部の高沸点成分は排水ライン65を通って廃液タンクへ排出される。   The component that condenses in the first packing 41 located at the lowest position is a high boiling point component such as water, which is stored in a liquid state at the bottom of the distillation column 40. The accumulated liquid is sent to the reboiler 59 where it is indirectly heated to become steam, returns to the bottom of the distillation column 40, and rises in the distillation column 40. In addition, some high-boiling components are discharged to the waste liquid tank through the drain line 65.

なお、装置の立ち上げ直後に第2水蒸気供給ライン60から蒸留塔40の底部に水蒸気を供給すれば、蒸発缶10からの蒸気が蒸留塔40内に充満するのを待たずに蒸留塔40の内部の温度を上昇させることができる。これにより、蒸留開始までにかかる時間を短縮することができる。また、メンテナンスの際に蒸留塔40内に水蒸気を直接供給すれば、蒸留塔40内を洗浄することもできる。   If water vapor is supplied from the second water vapor supply line 60 to the bottom of the distillation column 40 immediately after the start-up of the apparatus, the distillation column 40 is not waited for the vapor from the evaporator 10 to fill the distillation column 40. The internal temperature can be raised. Thereby, the time taken to start distillation can be shortened. Moreover, if water vapor | steam is directly supplied in the distillation column 40 in the case of a maintenance, the inside of the distillation column 40 can also be wash | cleaned.

一方、蒸発缶10で濃縮された廃溶剤は、固形成分を排出するために、廃溶剤抜き出しライン14を通って分離槽20に送られる。このとき、廃溶剤抜き出しバルブ15の開閉方法は廃溶剤に含まれる固形成分の性質によって適宜変更する。例えば、固形成分が互いに結合しやすい場合や高い粘着性を有する場合などには、固形成分同士が近づくのを避けるために、廃溶剤抜き出しバルブ15をタイマー制御により間欠的に開放しながら廃溶剤を流下させる。また、固形成分が廃溶剤中に漂いやすい場合などでは廃溶剤抜き出しバルブ15をわずかに開けて廃溶剤をゆっくりと連続的に流下させる。なお、廃溶剤抜き出しライン14の管内壁に固形成分が固着して管が閉塞した場合には、廃溶剤抜き出しバルブ15を閉じた状態で圧縮空気供給ライン16から圧縮空気を間欠的に管内に送ることにより、固着した固形成分を分離槽20へ押し流す。   On the other hand, the waste solvent concentrated in the evaporator 10 is sent to the separation tank 20 through the waste solvent extraction line 14 in order to discharge the solid components. At this time, the opening / closing method of the waste solvent extraction valve 15 is appropriately changed according to the properties of the solid components contained in the waste solvent. For example, when the solid components are easily bonded to each other or have high adhesiveness, the waste solvent is removed while the waste solvent extraction valve 15 is opened intermittently by timer control in order to prevent the solid components from approaching each other. Let it flow down. Further, when the solid component tends to drift in the waste solvent, the waste solvent extraction valve 15 is slightly opened to allow the waste solvent to flow slowly and continuously. When the solid component adheres to the inner wall of the waste solvent extraction line 14 and the tube is blocked, compressed air is intermittently sent from the compressed air supply line 16 into the tube with the waste solvent extraction valve 15 closed. As a result, the solid component that has adhered is pushed away into the separation tank 20.

分離槽20に流入する廃溶剤は、蒸発缶10で加熱されたものであるため、分離槽20に流入したときにその一部が蒸気になりやすい。この蒸気は廃溶液コンデンサ22において凝縮されて液体となるため、外部に漏れ出して大気を汚染するということがない。分離槽20に溜まった廃溶剤は沈降分離され、固形成分を含まない上澄液と、固形成分と溶剤成分が混じり合ったスラリーに分かれる。上澄液は第1〜第3上澄液流出口25〜27のうちのいずれかからオーバーフローし、上澄液流出ライン28を通って一時貯留槽29へ送られる。このとき、各上澄液流出口の設置高さには差を設けてあるため、分離槽20に流入する廃溶剤の量の変動に対応したり、分離槽20内の固形成分の濃度を調節したりすることができる。一時貯留槽29に溜まった上澄液は、ポンプ31により汲み上げられ、上澄液循環ライン30を通って蒸発缶10に戻る。このとき、上澄液を蒸発缶10に戻すのではなく廃液ライン34から廃液タンクへ排出することもできる。一方、分離槽20の底部に溜まったスラリーは、分離槽20における固形成分の割合が所定の値(例えば70%程度)まで高まったときに、分離槽20の下方に設けたドラム缶21に排出される。なお、一般的に廃溶剤に含まれる固形成分は溶剤成分よりも密度が高いため、廃溶剤中に漂いやすいものであっても分離槽20内で暫く静置することにより沈降する。   Since the waste solvent that flows into the separation tank 20 is heated by the evaporator 10, a part of the waste solvent tends to become vapor when it flows into the separation tank 20. Since this vapor is condensed in the waste solution condenser 22 to become a liquid, it does not leak outside and pollute the atmosphere. The waste solvent accumulated in the separation tank 20 is settled and separated into a supernatant liquid containing no solid component and a slurry in which the solid component and the solvent component are mixed. The supernatant overflows from any one of the first to third supernatant outlets 25 to 27, and is sent to the temporary storage tank 29 through the supernatant outlet line 28. At this time, since there is a difference in the installation height of each supernatant liquid outlet, it corresponds to fluctuations in the amount of waste solvent flowing into the separation tank 20, or the concentration of solid components in the separation tank 20 is adjusted. You can do it. The supernatant liquid collected in the temporary storage tank 29 is pumped up by the pump 31 and returns to the evaporator 10 through the supernatant circulation line 30. At this time, the supernatant liquid can be discharged from the waste liquid line 34 to the waste liquid tank instead of being returned to the evaporator 10. On the other hand, the slurry accumulated at the bottom of the separation tank 20 is discharged to a drum can 21 provided below the separation tank 20 when the ratio of solid components in the separation tank 20 increases to a predetermined value (for example, about 70%). The In general, since the solid component contained in the waste solvent has a higher density than the solvent component, even if the solid component is likely to drift in the waste solvent, it settles by being left in the separation tank 20 for a while.

本実施例に係る蒸留装置を用いて、固体成分を含有する廃溶剤からその廃溶剤の主成分であるアセトンを回収した例を説明する。使用した廃溶剤は、アセトン86.6wt%、水12.9wt%、レジスト等の高い粘着性を有する固形成分0.5wt%、メタノール200ppmを含んでいた。まず、蒸発缶10に廃溶剤を431kg/hで連続供給し、加熱部12により加熱しながら液体成分(アセトン、水、メタノール)を気化させた。このとき、廃溶剤抜き出しバルブ15は閉めておいた。暫く加熱を続け廃溶剤を濃縮し、廃溶剤に含まれる固形成分の濃度が約8wt%になった後、廃溶剤抜き出しバルブ15をタイマー制御で間欠的に開閉して、濃縮された廃溶剤を29kg/hの割合で分離槽20に抜き出した。抜き出した廃溶剤は、アセトン33.4wt%、水59.0wt%、固形成分7.6wt%、メタノール200ppmを含んでいた。   The example which collect | recovered acetone which is the main component of the waste solvent from the waste solvent containing a solid component using the distillation apparatus which concerns on a present Example is demonstrated. The waste solvent used contained 86.6 wt% acetone, 12.9 wt% water, 0.5 wt% solid component having high tackiness such as resist, and 200 ppm methanol. First, the waste solvent was continuously supplied to the evaporator 10 at 431 kg / h, and liquid components (acetone, water, methanol) were vaporized while being heated by the heating unit 12. At this time, the waste solvent extraction valve 15 was closed. Continue heating for a while and concentrate the waste solvent. After the concentration of the solid component in the waste solvent reaches about 8 wt%, the waste solvent extraction valve 15 is opened and closed intermittently under the timer control to remove the concentrated waste solvent. It extracted into the separation tank 20 at a rate of 29 kg / h. The extracted waste solvent contained 33.4 wt% acetone, 59.0 wt% water, 7.6 wt% solid components, and 200 ppm methanol.

分離槽20では、抜き出した廃溶剤を沈降分離し、上澄液とスラリーに分離した。上澄液は第1上澄液流出口25から流出させ、一時貯留槽29に溜めた後、ポンプ31により蒸発缶10に戻した。スラリーは、分離槽20での沈降分離を暫く続けて固形成分の濃度が70wt%になったときに、ドラム缶21に抜き出した。   In the separation tank 20, the extracted waste solvent was settled and separated into a supernatant and a slurry. The supernatant was discharged from the first supernatant outlet 25 and stored in the temporary storage tank 29, and then returned to the evaporator 10 by the pump 31. The slurry was extracted into the drum 21 when the concentration of the solid component reached 70 wt% by continuing the sedimentation separation in the separation tank 20 for a while.

蒸発缶10で気化した蒸気は蒸気ライン32を通して蒸留塔40に送り分離した。アセトンを多く含む回収溶剤は第2サイドカット口55から抜き出し、回収ライン56に配置した溶剤クーラー62で20℃まで冷却し回収した。この回収溶剤に占める各液体の含有量は、アセトン99.85wt%、水0.15wt%、メタノール30ppm以下であり、回収量は1時間あたり347kgであった。このように、蒸発缶10に供給した廃溶剤に含まれていたアセトンのうち92.8%という高い割合のアセトンを回収ライン56から回収することができた。   The vapor evaporated in the evaporator 10 was sent to the distillation column 40 through the vapor line 32 and separated. The recovered solvent containing a large amount of acetone was extracted from the second side cut port 55, cooled to 20 ° C. with a solvent cooler 62 disposed in the recovery line 56, and recovered. The content of each liquid in the recovered solvent was 99.85 wt% acetone, 0.15 wt% water, 30 ppm or less methanol, and the recovered amount was 347 kg per hour. Thus, a high proportion of 92.8% of acetone contained in the waste solvent supplied to the evaporator 10 could be recovered from the recovery line 56.

蒸留塔40の塔頂部にまで到達した溶剤は抜き出しライン53から抜き出した。このように抜き出した溶剤に占める各成分の含有量は、アセトン99.6wt%、メタノール0.4%であり、回収量は1時間あたり17kgであった。また、蒸留塔40の底部からは排水ライン65により1時間あたり38kgの水を廃液タンクに排出した。   The solvent that reached the top of the distillation column 40 was extracted from the extraction line 53. The content of each component in the extracted solvent was 99.6 wt% acetone and 0.4% methanol, and the recovered amount was 17 kg per hour. Further, 38 kg of water per hour was discharged from the bottom of the distillation tower 40 to the waste liquid tank through the drainage line 65.

本発明の一実施例である蒸留装置の概略構成図1 is a schematic configuration diagram of a distillation apparatus according to an embodiment of the present invention. 蒸留塔40内に設置した第1液分散装置45の縦断面図Longitudinal sectional view of the first liquid dispersion device 45 installed in the distillation tower 40 下側分散管74の平面図(a)及び上側分散管75の平面図(b)A plan view of the lower dispersion pipe 74 (a) and a plan view of the upper dispersion pipe 75 (b)

符号の説明Explanation of symbols

10…蒸発缶
11…廃溶剤供給ライン
12…加熱部
13…第1水蒸気供給ライン
14…廃溶剤抜き出しライン
15…廃溶剤抜き出しバルブ
16…圧縮空気供給ライン
20…分離槽
21…ドラム缶
22…廃溶液コンデンサ
23…凝縮ライン
24…スラリー抜き出しライン
25…第1上澄液流出口
26…第2上澄液流出口
27…第3上澄液流出口
28…上澄液流出ライン
29…一時貯留槽
30…上澄液循環ライン
31…ポンプ
32…蒸気ライン
33…ワイヤーメッシュデミスタ
34…廃液ライン
35…スラリー抜き出しバルブ
40…蒸留塔
41…第1充填物
42…第2充填物
43…第3充填物
44…第4充填物
45…第1液分散装置
46…第2液分散装置
47…第3液分散装置
48…第4液分散装置
49…精製物コンデンサ
50…第1パイプ
51…第2パイプ
52…第3パイプ
53…抜き出しライン
54…第1サイドカット口
55…第2サイドカット口
56…回収ライン
58…バイパスライン
59…リボイラ
60…第2水蒸気供給ライン
61…排水ポンプ
62…溶剤クーラー
63…再加熱ライン
65…排水ライン
66…連結部
71…コレクタ
72…内側筒部
73…外側筒部
74…下側分散管
75…上側分散管
76…細孔
77、79…中央パイプ
78、80…分枝パイプ
81…細孔
DESCRIPTION OF SYMBOLS 10 ... Evaporator 11 ... Waste solvent supply line 12 ... Heating part 13 ... 1st water vapor supply line 14 ... Waste solvent extraction line 15 ... Waste solvent extraction valve 16 ... Compressed air supply line 20 ... Separation tank 21 ... Drum can 22 ... Waste solution Capacitor 23 ... Condensation line 24 ... Slurry extraction line 25 ... First supernatant outlet 26 ... Second supernatant outlet 27 ... Third supernatant outlet 28 ... Supernatant outlet 29 ... Temporary storage tank 30 ... Supernatant circulation line 31 ... Pump 32 ... Steam line 33 ... Wire mesh demister 34 ... Waste liquid line 35 ... Slurry extraction valve 40 ... Distillation tower 41 ... First packing 42 ... Second packing 43 ... Third packing 44 ... the fourth filling 45 ... the first liquid dispersion device 46 ... the second liquid dispersion device 47 ... the third liquid dispersion device 48 ... the fourth liquid dispersion device 49 ... the purified product capacitor 50 ... the first pipe 51 Second pipe 52 ... Third pipe 53 ... Extraction line 54 ... First side cut port 55 ... Second side cut port 56 ... Recovery line 58 ... Bypass line 59 ... Reboiler 60 ... Second steam supply line 61 ... Drain pump 62 ... Solvent cooler 63 ... reheating line 65 ... drainage line 66 ... connecting part 71 ... collector 72 ... inner cylinder part 73 ... outer cylinder part 74 ... lower dispersion pipe 75 ... upper dispersion pipe 76 ... pores 77, 79 ... central pipe 78 80 ... branch pipe 81 ... pore

Claims (14)

固形成分を含有する廃溶剤から溶剤成分を回収する蒸留装置において、
前記廃溶剤を加熱して溶剤成分を気化させる蒸発器と、
前記蒸発器から前記廃溶剤を流出させる廃溶剤ラインと、
前記廃溶剤ラインから前記廃溶剤を受け、該廃溶剤を沈降分離する分離槽と、
前記分離槽で沈降分離された廃溶剤の上澄液を前記蒸発器に戻す上澄液ラインと、
を備えることを特徴とする蒸留装置。
In a distillation apparatus that recovers a solvent component from a waste solvent containing a solid component,
An evaporator for heating the waste solvent to vaporize a solvent component;
A waste solvent line for draining the waste solvent from the evaporator;
A separation tank for receiving the waste solvent from the waste solvent line and settling and separating the waste solvent;
A supernatant line for returning the supernatant of the waste solvent settled and separated in the separation tank to the evaporator;
A distillation apparatus comprising:
前記分離槽が前記蒸発器の下方に設けられるとともに、前記廃溶剤ラインの一端が前記蒸発器の底部に接続することを特徴とする請求項1に記載の蒸留装置。   2. The distillation apparatus according to claim 1, wherein the separation tank is provided below the evaporator, and one end of the waste solvent line is connected to the bottom of the evaporator. 前記廃溶剤ラインを流れる廃溶剤の流量調整手段を備えることを特徴とする請求項1又は2に記載の蒸留装置。   The distillation apparatus according to claim 1, further comprising a flow rate adjusting unit for waste solvent flowing through the waste solvent line. 前記廃溶剤ラインの管内に圧縮空気を送る圧縮空気供給手段を備えることを特徴とする請求項1〜3のいずれかに記載の蒸留装置。   The distillation apparatus according to any one of claims 1 to 3, further comprising compressed air supply means for sending compressed air into a pipe of the waste solvent line. 前記分離槽における上澄液の流出口が、前記分離槽の壁面の異なる高さ位置に複数設けられることを特徴とする請求項1〜4のいずれかに記載の蒸留装置。   The distillation apparatus according to any one of claims 1 to 4, wherein a plurality of supernatant outlets in the separation tank are provided at different height positions on the wall surface of the separation tank. 前記分離槽内の廃溶剤蒸気を凝縮させる凝縮手段を備えることを特徴とする請求項1〜5のいずれかに記載の蒸留装置。   The distillation apparatus according to claim 1, further comprising a condensing unit that condenses the waste solvent vapor in the separation tank. 前記蒸発器内の廃溶剤を水蒸気の熱により間接加熱する加熱部を有するとともに、該加熱部に水蒸気を供給する水蒸気供給ラインが該加熱部だけでなく前記蒸発器内にも適宜水蒸気を供給することを特徴とする請求項1〜6のいずれかに記載の蒸留装置。   A heating unit that indirectly heats the waste solvent in the evaporator with the heat of water vapor, and a water vapor supply line that supplies water vapor to the heating unit appropriately supplies water vapor not only to the heating unit but also to the evaporator. The distillation apparatus according to any one of claims 1 to 6. 前記蒸発器における廃溶剤蒸気の出口に、廃溶剤に含まれる固形成分の通り抜けを阻止する固形成分除去手段を備えることを特徴とする請求項1〜7のいずれかに記載の蒸留装置。   The distillation apparatus according to any one of claims 1 to 7, further comprising a solid component removing unit that prevents passage of solid components contained in the waste solvent at an outlet of the waste solvent vapor in the evaporator. 前記蒸発器より流入する廃溶剤蒸気を沸点の違いを利用して分離する蒸留部を備えるとともに、該蒸留部がサイドカット方式により精製物を留出するサイドカット口を備えることを特徴とする請求項1〜8のいずれかに記載の蒸留装置。   A distillation section that separates waste solvent vapor flowing from the evaporator using a difference in boiling point, and the distillation section includes a side cut port for distilling a purified product by a side cut method. Item 9. The distillation apparatus according to any one of Items 1 to 8. 前記サイドカット口を複数備え、前記蒸留部における異なる温度領域から精製物を留出することを特徴とする請求項9に記載の蒸留装置。   The distillation apparatus according to claim 9, comprising a plurality of the side cut ports, and distilling the purified product from different temperature ranges in the distillation section. 前記蒸留部の上部から留出する精製物を凝縮させて該蒸留部に戻す還流ラインと、
前記サイドカット口から留出する精製物を冷却して回収する回収ラインと、
前記還流ラインにて凝縮した精製物を前記回収ラインに送るバイパスラインと、
を備えることを特徴とする請求項9又は10に記載の蒸留装置。
A reflux line for condensing the purified product distilled from the upper part of the distillation part and returning it to the distillation part;
A recovery line for cooling and recovering the purified product distilled from the side cut port;
A bypass line for sending the purified product condensed in the reflux line to the recovery line;
The distillation apparatus according to claim 9 or 10, comprising:
前記蒸発器より流入する廃溶剤蒸気を沸点の違いを利用して分離する蒸留部を備えるとともに、該蒸留部の内部に、上方より供給される液体を下方に分散供給する液分散手段を備えることを特徴とする請求項1〜11のいずれかに記載の蒸留装置。   A distillation unit that separates waste solvent vapor flowing in from the evaporator by utilizing a difference in boiling point, and a liquid dispersion unit that supplies and supplies a liquid supplied from above downward in the distillation unit. The distillation apparatus according to claim 1, wherein: 前記液分散手段が、
上方より供給される液体を集めて下方に流出するコレクタと、
前記コレクタの下方に設けられ、前記コレクタにて集められた液体を導入する内側筒部と、
前記内側筒部の外側に、前記内側筒部との間に隙間を空けて設けられた外側筒部と、
前記内側筒部の下部と接続し、水平面内で枝分かれする複数の下側分枝パイプを有し、前記内側筒部の内側を流れる液体を導入して前記下側分枝パイプの底部に設けた細孔から液体を流下する下側分散管と、
前記外側筒部の下部と接続し、水平面内で枝分かれする複数の上側分枝パイプを有し、前記外側筒部と前記内側筒部の間の隙間を流れる液体を導入して前記上側分枝パイプの底部に設けた細孔から液体を流下する上側分散管と、
を備えることを特徴とする請求項12に記載の蒸留装置。
The liquid dispersing means is
A collector that collects liquid supplied from above and flows downward;
An inner cylindrical portion that is provided below the collector and introduces liquid collected by the collector;
An outer cylinder provided outside the inner cylinder with a gap between the inner cylinder and the inner cylinder;
A plurality of lower branch pipes connected to the lower part of the inner cylinder part and branched in a horizontal plane are provided at the bottom of the lower branch pipe by introducing a liquid flowing inside the inner cylinder part A lower dispersion tube for flowing liquid from the pores;
A plurality of upper branch pipes connected to the lower part of the outer cylinder part and branched in a horizontal plane, and the upper branch pipe is introduced by introducing a liquid flowing in a gap between the outer cylinder part and the inner cylinder part An upper dispersion pipe for flowing the liquid from the pores provided at the bottom of
The distillation apparatus according to claim 12, comprising:
前記蒸発器より流入する廃溶剤蒸気を沸点の違いを利用して分離する蒸留部を備えるとともに、該蒸留部の底部に溜まった液体を水蒸気の熱により間接加熱する再加熱手段を備え、該再加熱手段に水蒸気を供給する水蒸気供給ラインが該再加熱手段だけでなく前記蒸留部の底部にも適宜水蒸気を供給することを特徴とする請求項1〜13のいずれかに記載の蒸留装置。   A distillation unit that separates waste solvent vapor flowing from the evaporator by utilizing a difference in boiling point; and a reheating unit that indirectly heats the liquid accumulated at the bottom of the distillation unit by the heat of water vapor. The distillation apparatus according to any one of claims 1 to 13, wherein a water vapor supply line for supplying water vapor to the heating means appropriately supplies water vapor not only to the reheating means but also to the bottom of the distillation section.
JP2007278260A 2007-10-26 2007-10-26 Distilling apparatus of waste solvent containing solid component Pending JP2009101334A (en)

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CN111114969A (en) * 2020-02-03 2020-05-08 余娅君 Dual-mode distilled liquid storage device
CN113813633A (en) * 2021-09-29 2021-12-21 聊城鲁西氯甲烷化工有限公司 Chloroform rectification device and rectification process
KR20230011727A (en) * 2021-07-14 2023-01-25 티이엠씨 주식회사 System and method for solvent recovery in the diborane manufacturing process

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105892337A (en) * 2014-12-15 2016-08-24 广西大学 Tumbler-type tank device control system
CN105892337B (en) * 2014-12-15 2018-07-03 广西大学 A kind of clear tank arrangement control system of pivoted arm
KR20190134773A (en) * 2017-04-13 2019-12-04 사이펨 에스.피.에이. Liquid dual dispensing device especially used in devices in which the liquid state flows under gravity.
JP2020516451A (en) * 2017-04-13 2020-06-11 サイペム エスピーアー Liquid dual distributor, especially for use in devices in which the liquid phase flows under gravity
JP7117319B2 (en) 2017-04-13 2022-08-12 サイペム エスピーアー A dual liquid distributor suitable for use in devices where the liquid phase flows under gravity
KR102504035B1 (en) 2017-04-13 2023-02-28 사이펨 에스.피.에이. Liquid double dispensing device, especially used in apparatuses where the liquid state flows under gravity.
CN111114969A (en) * 2020-02-03 2020-05-08 余娅君 Dual-mode distilled liquid storage device
CN111114969B (en) * 2020-02-03 2020-11-13 烟台海市葡萄酒有限公司 Dual-mode distilled liquid storage device
KR20230011727A (en) * 2021-07-14 2023-01-25 티이엠씨 주식회사 System and method for solvent recovery in the diborane manufacturing process
KR102581029B1 (en) 2021-07-14 2023-09-22 티이엠씨 주식회사 System and method for solvent recovery in the diborane manufacturing process
CN113813633A (en) * 2021-09-29 2021-12-21 聊城鲁西氯甲烷化工有限公司 Chloroform rectification device and rectification process

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