TW201925145A - Solvent dehydration system and solvent dehydration method - Google Patents

Solvent dehydration system and solvent dehydration method Download PDF

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TW201925145A
TW201925145A TW107141125A TW107141125A TW201925145A TW 201925145 A TW201925145 A TW 201925145A TW 107141125 A TW107141125 A TW 107141125A TW 107141125 A TW107141125 A TW 107141125A TW 201925145 A TW201925145 A TW 201925145A
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mixed liquid
pervaporation
solvent
mixture
solvent dehydration
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大川光治郎
澤村健一
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大川光治郎
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/36Pervaporation; Membrane distillation; Liquid permeation
    • B01D61/365Osmotic distillation or osmotic evaporation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/36Pervaporation; Membrane distillation; Liquid permeation
    • B01D61/362Pervaporation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/36Pervaporation; Membrane distillation; Liquid permeation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/36Pervaporation; Membrane distillation; Liquid permeation
    • B01D61/366Apparatus therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/36Pervaporation; Membrane distillation; Liquid permeation
    • B01D61/368Accessories; Auxiliary operations
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/10Supported membranes; Membrane supports
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/10Supported membranes; Membrane supports
    • B01D69/108Inorganic support material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12Composite membranes; Ultra-thin membranes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12Composite membranes; Ultra-thin membranes
    • B01D69/1213Laminated layers
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02Inorganic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2311/00Details relating to membrane separation process operations and control
    • B01D2311/10Temperature control
    • B01D2311/103Heating

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

An object of the present invention is to provide a solvent dehydration system and a solvent dehydration method, wherein the solvent dehydration system can supply the stable-temperature mixed liquid to the permeation vaporization device, and efficiently dehydrate the mixture. The present invention is characterized by a solvent dehydration system including a permeation vaporization device, a third supply path and a heating means. The permeation vaporization device is used for dehydrating mixed liquid including a water-soluble hydrocarbon solvent and water. The third supply path is used for supplying the mixed liquid to permeation vaporization device. The heating means is used for heating the mixed liquid supplied to the permeation vaporization device. The solvent dehydration system further includes a vacuum distillation regeneration device which is used for generating the mixed liquid. The vacuum distillation regeneration device passes through the second supply path and the third supply path to connect to the permeation vaporization device.

Description

溶劑脫水系統及溶劑脫水方法Solvent dehydration system and solvent dehydration method

本發明係關於一種將有機溶劑(例如用於洗淨有機發光二極體用的金屬遮罩)和水的混合液,分離為有機溶劑和水的溶劑脫水系統及溶劑脫水方法。The present invention relates to a solvent dehydration system and a solvent dehydration method for separating a mixture of an organic solvent (for example, a metal mask for washing an organic light-emitting diode) and water into an organic solvent and water.

例如,洗淨附著有機發光二極體用的有機材料之金屬遮罩等被洗淨物時,將被洗淨物多次浸漬到儲存於洗淨裝置的水溶性有機溶劑(例如烴類溶劑(HC)等),進行洗淨處理。For example, when washing a metal object such as a metal mask for an organic material for attaching an organic light-emitting diode, the object to be washed is immersed several times in a water-soluble organic solvent (for example, a hydrocarbon solvent) stored in the cleaning device. HC), etc., and washed.

由於這種水溶性有機溶劑容易吸收水分,例如隨著取出放入被洗淨物,可能使水的含有量因和空氣接觸而逐漸增加,降低其作為洗淨液的性能。於是,各種溶劑脫水技術被提出,以除去水溶性有機溶劑所吸收的水。Since such a water-soluble organic solvent easily absorbs moisture, for example, as it is taken out and put into the object to be washed, the content of water may gradually increase due to contact with air, and the performance as a cleaning liquid may be lowered. Thus, various solvent dehydration techniques have been proposed to remove water absorbed by the water-soluble organic solvent.

例如,專利文獻1記載的一種有機溶劑精製系統,其係包含:一脫氣裝置21,從水和有機溶劑的混合液去除氣體成分;一離子交換裝置11,從已脫氣的混合液去除離子雜質;一熱交換器12,將已去除離子雜質的混合液加熱;及一浸透汽化裝置13,將混合液分離為有機溶劑和水。藉此,專利文獻1具有優越的節能性能,同時可抑制氧化變質並從混合液分離出有機溶劑。For example, an organic solvent purification system described in Patent Document 1 includes a deaeration device 21 that removes a gas component from a mixture of water and an organic solvent, and an ion exchange device 11 that removes ions from the degassed mixture. Impurities; a heat exchanger 12 that heats the mixture of ionic impurities removed; and a pervaporation device 13 that separates the mixture into an organic solvent and water. Thereby, Patent Document 1 has superior energy-saving performance while suppressing oxidative deterioration and separating the organic solvent from the mixed liquid.

但,於上述的浸透汽化裝置中,為了有效率地分離有機溶劑和水,優選供給被加熱到適於浸透汽化的溫度之混合液。但,於專利文獻1,由於藉由使用蒸氣的熱交換器12加熱混合液,根據混合液的溫度或流速、及蒸氣的溫度,會產生供給到浸透汽化裝置的混合液之溫度不穩定的問題。因此,專利文獻1恐怕不能有效率地分離有機溶劑和水。However, in the above-described permeation vaporization apparatus, in order to efficiently separate the organic solvent and water, it is preferred to supply a mixed liquid heated to a temperature suitable for pervaporation. However, in Patent Document 1, since the mixed liquid is heated by the heat exchanger 12 using steam, the temperature of the mixed liquid supplied to the vaporization device is unstable depending on the temperature or flow rate of the mixed liquid and the temperature of the vapor. . Therefore, Patent Document 1 may not efficiently separate the organic solvent and water.

專利文獻Patent literature

專利文獻1: 特開2016-030232號公報Patent Document 1: JP-A-2016-030232

有鑑於上述問題,本發明的目的是提供一種將溫度穩定的混合液供給到浸透汽化裝置且能有效率地將混合液脫水的溶劑脫水系統及溶劑脫水方法。In view of the above problems, an object of the present invention is to provide a solvent dehydration system and a solvent dehydration method which supply a temperature-stable mixed liquid to a pervaporation apparatus and can efficiently dehydrate the mixture.

本發明的特徵是一種溶劑脫水系統,其係包含:一浸透汽化裝置,將水溶性有機溶劑和水的混合液脫水;一供給路徑,將混合液供給到浸透汽化裝置;及一加熱手段,將供給到浸透汽化裝置的混合液加熱;其中,溶劑脫水系統更包含一生成混合液的蒸餾再生裝置,蒸餾再生裝置經由供給路徑連接到浸透汽化裝置。The present invention is characterized by a solvent dehydration system comprising: a pervaporation device for dehydrating a mixture of a water-soluble organic solvent and water; a supply path for supplying the mixture to the pervaporation device; and a heating means The mixture supplied to the vaporization device is heated; wherein the solvent dehydration system further comprises a distillation regeneration device for generating a mixed liquid, and the distillation regeneration device is connected to the pervaporation device via a supply path.

又,本發明的特徵是一種溶劑脫水方法,其使用的系統包含:一浸透汽化裝置,將水溶性有機溶劑和水的混合液脫水;一供給路徑,將混合液供給到浸透汽化裝置;及一加熱手段,將供給到浸透汽化裝置的混合液加熱;其中,溶劑脫水方法包含:一蒸餾再生裝置生成混合液的步驟;一用加熱手段加熱混合液的步驟;一經由供給路徑將混合液從蒸餾再生裝置供給到浸透汽化裝置的步驟;及一用浸透汽化裝置將混合液脫水的步驟。Further, the present invention features a solvent dehydration method using a system comprising: a pervaporation device for dehydrating a mixture of a water-soluble organic solvent and water; a supply path for supplying the mixture to the pervaporation device; Heating means, heating the mixed liquid supplied to the vaporization device; wherein the solvent dehydration method comprises: a step of generating a mixed liquid by the distillation regeneration device; a step of heating the mixed liquid by heating means; and discharging the mixed liquid from the distillation path through the supply path a step of supplying the regeneration device to the pervaporation device; and a step of dehydrating the mixture with the pervaporation device.

上述有機溶劑,例如為水溶性的烴類溶劑(HC)等,具體來說,其係具有吸濕性的N-甲基-2-吡咯烷酮(NMP)等。藉由本發明,溶劑脫水系統及溶劑脫水方法,可將溫度穩定的混合液供給到浸透汽化裝置,有效率地將混合液脫水。具體來說,蒸餾再生裝置將含有雜質的混合液汽化蒸發後,藉由冷卻生成已去除雜質的混合液。The organic solvent is, for example, a water-soluble hydrocarbon solvent (HC), and specifically, a hygroscopic N-methyl-2-pyrrolidone (NMP) or the like. According to the present invention, the solvent dehydration system and the solvent dehydration method can supply a temperature-stable mixed liquid to the permeation vaporization device, and the mixture can be efficiently dehydrated. Specifically, the distillation regeneration device vaporizes and vaporizes the mixed solution containing the impurities, and then forms a mixed liquid from which impurities have been removed by cooling.

因此,蒸餾再生裝置可容易地排出溫度較高且溫度穩定的混合液。藉此,溶劑脫水系統及溶劑脫水方法,可容易且穩定地將溫度較高的混合液供給到浸透汽化裝置。Therefore, the distillation regeneration apparatus can easily discharge the mixed liquid having a relatively high temperature and a stable temperature. Thereby, the solvent dehydration system and the solvent dehydration method can easily and stably supply the mixed liquid having a relatively high temperature to the pervaporation vaporization device.

進一步地,例如即使蒸餾再生裝置排出溫度高於常溫且低於適於浸透汽化的溫度之混合液,藉由用加熱手段加熱混合液,溶劑脫水系統及溶劑脫水方法,可快速地用較少的熱能將混合液加熱到所需的溫度。Further, for example, even if the distillation regeneration device discharges a mixture having a temperature higher than a normal temperature and lower than a temperature suitable for pervaporation, by heating the mixture by heating means, the solvent dehydration system and the solvent dehydration method, it is possible to quickly use less Thermal energy heats the mixture to the desired temperature.

或,藉由蒸餾再生裝置直接將溫度適於浸透汽化的混合液供給到浸透汽化裝置,溶劑脫水系統及溶劑脫水方法,可使用蒸餾再生裝置作為加熱手段,將供給到浸透汽化裝置的混合液加熱。Alternatively, the mixture is supplied to the pervaporation device, the solvent dehydration system and the solvent dehydration method by directly supplying the mixed solution having a temperature suitable for pervaporation by a distillation regeneration device, and the distillation regenerative device can be used as a heating means to heat the mixture supplied to the pervaporation device. .

由於在這種情況下,溶劑脫水系統及溶劑脫水方法,例如可不需要使用蒸氣的熱交換器、及將蒸汽供給到熱交換器的裝置,故可用簡單的構造有效率地將混合液脫水。因此,溶劑脫水系統及溶劑脫水方法,可將溫度穩定的混合液供給到浸透汽化裝置,有效率地將混合液脫水。In this case, the solvent dehydration system and the solvent dehydration method, for example, a heat exchanger using steam and a device for supplying steam to the heat exchanger can be omitted, so that the mixed liquid can be efficiently dehydrated with a simple structure. Therefore, the solvent dehydration system and the solvent dehydration method can supply a temperature-stable mixed liquid to the permeation vaporization device, and efficiently dehydrate the mixed liquid.

作為本發明的實施方式,其構成係讓蒸餾再生裝置和浸透汽化裝置之間係包含:一暫時儲存槽,暫時儲存供給到浸透汽化裝置的混合液;及一預熱手段;預熱儲存在暫時儲存槽的混合液;其中,加熱手段係加熱從暫時儲存槽供給到浸透汽化裝置的混合液。As an embodiment of the present invention, the configuration is such that the distillation regeneration device and the pervaporation vaporization device comprise: a temporary storage tank for temporarily storing the mixed liquid supplied to the vaporization device; and a preheating means; the preheating is temporarily stored a mixed solution of the storage tank; wherein the heating means heats the mixed liquid supplied from the temporary storage tank to the vaporization device.

藉由本發明,例如即使在有機溶劑的引火點低於蒸餾再生裝置的蒸餾溫度之情況下,溶劑脫水系統也可安全地將溫度穩定的混合液供給到浸透汽化裝置。具體來說,在有機溶劑的引火點低於蒸餾溫度的情況下,若從蒸餾再生裝置排出高溫的混合液,會提高引火的危險性。According to the present invention, for example, even in the case where the ignition point of the organic solvent is lower than the distillation temperature of the distillation regeneration apparatus, the solvent dehydration system can safely supply the temperature-stable mixed liquid to the pervaporation vaporization apparatus. Specifically, when the ignition point of the organic solvent is lower than the distillation temperature, if the high-temperature mixed liquid is discharged from the distillation regeneration device, the risk of ignition is increased.

在這種情況下,蒸餾再生裝置,其構成係讓混合液冷卻到低於有機溶劑的引火點之溫度(例如常溫)再排出。因此,若只用加熱手段加熱混合液,恐怕無法將溫度穩定的混合液供給到浸透汽化裝置。In this case, the distillation regenerating apparatus is configured such that the mixed liquid is cooled to a temperature lower than the ignition point of the organic solvent (for example, normal temperature) and discharged. Therefore, if the mixed liquid is heated only by heating means, it is feared that the temperature-stable mixed liquid cannot be supplied to the pervaporation vaporization device.

於是,溶劑脫水系統藉由包含:一暫時儲存槽,暫時儲存供給到浸透汽化裝置的混合液;及一預熱手段;預熱所儲存的混合液,例如可在將常溫的混合液供給到浸透汽化裝置之前預熱到預定溫度。因此,相較於直接將混合液從蒸餾再生裝置供給到浸透汽化裝置的情況,溶劑脫水系統可更安全地將混合液供給到浸透汽化裝置。Thus, the solvent dehydration system temporarily stores the mixed liquid supplied to the vaporization device by a temporary storage tank; and a preheating means; preheating the stored mixed liquid, for example, supplying the mixed liquid at normal temperature to the saturated solution The vaporizer is preheated to a predetermined temperature. Therefore, the solvent dehydration system can supply the mixed liquid to the pervaporation apparatus more safely than the case where the mixed liquid is directly supplied from the distillation regeneration device to the pervaporation vaporization device.

進一步地,藉由用加熱手段加熱已預熱的混合液,溶劑脫水系統可快速地用較少的熱能將混合液加熱到所需的溫度。因此,溶劑脫水系統可將溫度更穩定的混合液供給到浸透汽化裝置。因此,例如即使在有機溶劑的引火點低於蒸餾再生裝置的蒸餾溫度之情況下,溶劑脫水系統也可安全地將溫度穩定的混合液供給到浸透汽化裝置。Further, by heating the preheated mixture with heating, the solvent dewatering system can quickly heat the mixture to the desired temperature with less heat. Therefore, the solvent dehydration system can supply a more stable temperature mixture to the pervaporation vaporizer. Therefore, for example, even in the case where the ignition point of the organic solvent is lower than the distillation temperature of the distillation regeneration apparatus, the solvent dehydration system can safely supply the temperature-stable mixed liquid to the pervaporation vaporization apparatus.

又,作為本發明的實施方式,浸透汽化裝置包含:一浸透汽化膜組件,其係用於將混合液脫水;其中,浸透汽化膜組件係由多孔陶瓷支持體和微多孔陶瓷分離膜的積層體所構成。上述微多孔陶瓷分離膜係指沸石分離膜、二氧化矽分離膜、碳分離膜等。藉由本發明,溶劑脫水系統藉由溫度穩定的混合液和浸透汽化膜組件,可有效率且更穩定地分離有機溶劑和水。Further, as an embodiment of the present invention, the pervaporation vaporization apparatus comprises: a permeation vaporization membrane module for dehydrating the mixture; wherein the pervaporation membrane module is a laminate of the porous ceramic support and the microporous ceramic separation membrane. Composition. The microporous ceramic separation membrane refers to a zeolite separation membrane, a ceria separation membrane, a carbon separation membrane, and the like. By the present invention, the solvent dehydration system can efficiently and more stably separate the organic solvent and water by the temperature-stable mixture and the pervaporation membrane module.

又,作為本發明的實施方式,包含:一洗淨裝置,用有機溶劑去除附著於被洗淨物的附著物;一送液路徑,將於洗淨裝置生成的雜質、水及有機溶劑之混合液從洗淨裝置送到蒸餾再生裝置;及一回流路徑,將用浸透汽化裝置脫水過的有機溶劑回流到洗淨裝置。藉由本發明,溶劑脫水系統可將用浸透汽化裝置脫水過的有機溶劑反覆利用於被洗淨物的洗淨。Further, an embodiment of the present invention includes: a cleaning device that removes an adhering matter attached to the object to be washed with an organic solvent; and a liquid supply path that mixes impurities, water, and an organic solvent generated in the cleaning device. The liquid is sent from the cleaning device to the distillation regeneration device; and a reflux path is used to reflux the organic solvent dehydrated by the vaporization device to the cleaning device. According to the present invention, the solvent dehydration system can repeatedly use the organic solvent dehydrated by the pervaporation apparatus to wash the washed matter.

藉由本發明,可提供一種將溫度穩定的混合液供給到浸透汽化裝置且能有效率地將混合液脫水的溶劑脫水系統及溶劑脫水方法。According to the present invention, it is possible to provide a solvent dehydration system and a solvent dehydration method which supply a temperature-stable mixed liquid to a pervaporation vaporization apparatus and can efficiently dehydrate the mixed liquid.

與以下圖式一同說明本發明的一實施方式。首先,用圖1及圖2說明本實施方式的溶劑脫水系統1。且,圖1所示為溶劑脫水系統1的構成圖,圖2所示為浸透汽化裝置40的裝置主體部41的構成圖。An embodiment of the present invention will be described together with the following drawings. First, the solvent dehydration system 1 of the present embodiment will be described with reference to Figs. 1 and 2 . 1 is a configuration diagram of the solvent dehydration system 1, and FIG. 2 is a configuration diagram of the apparatus main body portion 41 which is impregnated into the vaporization device 40.

如圖1所示,溶劑脫水系統1,由一用烴類溶劑(HC)S(其係水溶性有機溶劑)洗淨被洗淨物之洗淨裝置10;一從烴類溶劑和水和雜質的混合液X1去除雜質之真空蒸餾再生裝置20;一用預定溫度預熱已去除雜質的混合液X2之預熱槽30;及一將已預熱的混合液X2脫水之浸透汽化裝置40所構成。As shown in Fig. 1, the solvent dehydration system 1 is a cleaning device 10 for washing the washed matter with a hydrocarbon solvent (HC) S (which is a water-soluble organic solvent); a hydrocarbon solvent and water and impurities. a vacuum distillation regeneration device 20 for removing impurities from the mixture X1; a preheating tank 30 for preheating the mixed liquid X2 from which impurities have been removed by a predetermined temperature; and a pervaporation device 40 for dehydrating the preheated mixed liquid X2 .

進一步地,溶劑脫水系統1係包含:一第1供給路徑P1,將混合液X1從洗淨裝置10供給到真空蒸餾再生裝置20;一第2供給路徑P2,將混合液X2從真空蒸餾再生裝置20供給到預熱槽30;一第3供給路徑P3,將混合液X2從預熱槽30供給到浸透汽化裝置40;及一第4供給路徑P4,將烴類溶劑S從浸透汽化裝置40供給到洗淨裝置10。Further, the solvent dehydration system 1 includes a first supply path P1, the mixed liquid X1 is supplied from the cleaning device 10 to the vacuum distillation regeneration device 20, a second supply path P2, and the mixed liquid X2 is removed from the vacuum distillation regeneration device. 20 is supplied to the preheating tank 30; a third supply path P3, the mixed liquid X2 is supplied from the preheating tank 30 to the permeation vaporization device 40; and a fourth supply path P4, the hydrocarbon solvent S is supplied from the permeation vaporization device 40. Go to the cleaning device 10.

如圖1所示,洗淨裝置10是例如用水溶性的烴類溶劑S分成多次洗淨有機發光二極體的蒸鍍製程使用的金屬遮罩M,以去除有機材料等的雜質之裝置。且,作為水溶性的烴類溶劑S,其係具有吸濕性的N-甲基-2-吡咯烷酮(NMP)。具體來說,洗淨裝置10,由一第1洗淨部11、第2洗淨部12及第3洗淨部13所組成的3個洗淨部;一連接第2洗淨部12及第3洗淨部13的第1送液路徑14;及一連接第1洗淨部11及第2洗淨部12的第2送液路徑15所構成。且,雖省略詳細圖式,洗淨裝置10,其構成係按照第1洗淨部11、第2洗淨部12、第3洗淨部13的順序,運送及洗淨金屬遮罩M。As shown in Fig. 1, the cleaning device 10 is a device that removes impurities such as organic materials by dividing the metal mask M used in the vapor deposition process of the organic light-emitting diode by a water-soluble hydrocarbon solvent S, for example. Further, it is a water-soluble hydrocarbon solvent S which is hygroscopic N-methyl-2-pyrrolidone (NMP). Specifically, the cleaning device 10 includes three cleaning units including a first cleaning unit 11, a second cleaning unit 12, and a third cleaning unit 13, and a second cleaning unit 12 and a second unit. The first liquid supply path 14 of the cleaning unit 13 and the second liquid supply path 15 that connects the first cleaning unit 11 and the second cleaning unit 12. In addition, the cleaning apparatus 10 is configured to transport and clean the metal mask M in the order of the first cleaning unit 11, the second cleaning unit 12, and the third cleaning unit 13, although the detailed drawings are omitted.

第1洗淨部11,由一儲存烴類溶劑S的第1洗淨槽111;及一鄰近第1洗淨槽111而設的第1儲存槽112所構成。第1洗淨槽111,儲存著未使用、或雜質或水分較少的烴類溶劑S。The first cleaning unit 11 is composed of a first cleaning tank 111 for storing the hydrocarbon solvent S and a first storage tank 112 provided adjacent to the first cleaning tank 111. The first cleaning tank 111 stores a hydrocarbon solvent S which is not used or has less impurities or moisture.

進一步地,超音波振動器113設置在第1洗淨槽111的底部,用於對烴類溶劑S引起超音波振動。且,第1洗淨槽111,會在適當的時機從補充槽(省略圖式)補充未使用的烴類溶劑。Further, the ultrasonic vibrator 113 is provided at the bottom of the first cleaning tank 111 for causing ultrasonic vibration to the hydrocarbon solvent S. Further, the first cleaning tank 111 replenishes the unused hydrocarbon solvent from the replenishing tank (omitted from the drawing) at an appropriate timing.

第1儲存槽112,其構成係儲存從第1洗淨槽111溢出的混合液。且,此混合液是從金屬遮罩M分離出的有機材料等的雜質和從空氣中吸收的水分和烴類溶劑S之混合液。The first storage tank 112 has a configuration in which the mixed liquid overflowing from the first washing tank 111 is stored. Further, the mixed liquid is a mixture of impurities such as an organic material separated from the metal mask M and water and a hydrocarbon solvent S absorbed from the air.

第2洗淨部12,由一儲存烴類溶劑S的第2洗淨槽121;一鄰近第2洗淨槽121而設的第2儲存槽122;及一設置在第2洗淨槽121的底部之超音波振動器123所構成。且,由於第2洗淨槽121、第2儲存槽122及超音波振動器123與第1洗淨部11的構成相同,故省略其詳細說明。The second cleaning unit 12 includes a second cleaning tank 121 that stores the hydrocarbon solvent S, a second storage tank 122 that is adjacent to the second cleaning tank 121, and a second cleaning tank 121 that is disposed in the second cleaning tank 121. The bottom ultrasonic vibrator 123 is constructed. In addition, since the second cleaning tank 121, the second storage tank 122, and the ultrasonic vibrator 123 have the same configuration as that of the first cleaning unit 11, detailed description thereof will be omitted.

第3洗淨部13,由一儲存烴類溶劑S的第3洗淨槽131;一鄰近第3洗淨槽131而設的第3儲存槽132;及一設置在第3洗淨槽131的底部之超音波振動器133所構成。且,由於第3洗淨槽131、第3儲存槽132及超音波振動器133與第1洗淨部11的構成相同,故省略其詳細說明。The third cleaning unit 13 includes a third cleaning tank 131 that stores the hydrocarbon solvent S, a third storage tank 132 that is adjacent to the third cleaning tank 131, and a third cleaning tank 131 that is disposed in the third cleaning tank 131. The bottom ultrasonic vibrator 133 is constructed. Further, since the third cleaning tank 131, the third storage tank 132, and the ultrasonic vibrator 133 have the same configuration as that of the first cleaning unit 11, detailed description thereof will be omitted.

如圖1所示,第1送液路徑14,其構成係作為一流動路徑,將混合液從第3儲存槽132的液面附近送到第2儲存槽122的底部。如圖1所示,第2送液路徑15,其構成係作為一流動路徑,將混合液從第2儲存槽122的液面附近送到第1儲存槽112的底部。As shown in FIG. 1, the first liquid supply path 14 is configured as a flow path, and the mixed liquid is sent from the vicinity of the liquid surface of the third storage tank 132 to the bottom of the second storage tank 122. As shown in FIG. 1, the second liquid supply path 15 is configured as a flow path for supplying the mixed liquid from the vicinity of the liquid surface of the second storage tank 122 to the bottom of the first storage tank 112.

因此,第1洗淨部11的第1儲存槽112,儲存著從第1洗淨槽111溢出的混合液和從第2洗淨部12的儲存槽122及第3洗淨部13的第3儲存槽132送出的混合液之混合液X1。如圖1所示,上述構成的洗淨裝置10,經由連接到第1洗淨部11的第1儲存槽112的液面附近之第1供給路徑P1,連接到真空蒸餾再生裝置20。Therefore, the first storage tank 112 of the first cleaning unit 11 stores the mixed liquid overflowing from the first cleaning tank 111 and the storage tank 122 of the second cleaning unit 12 and the third cleaning unit 13 The mixed liquid X1 of the mixed liquid sent from the storage tank 132. As shown in FIG. 1, the cleaning apparatus 10 of the above-described configuration is connected to the vacuum distillation regeneration apparatus 20 via the first supply path P1 connected to the vicinity of the liquid surface of the first storage tank 112 of the first cleaning unit 11.

又,如圖1所示,真空蒸餾再生裝置20,由一具有略密閉的內部空間之蒸發槽21;一具有略密閉的內部空間之冷凝槽22;及一連結蒸發槽21的上部及冷凝槽22的上部之連通路徑23所構成。Further, as shown in FIG. 1, the vacuum distillation regenerating apparatus 20 includes an evaporation tank 21 having a slightly sealed internal space, a condensation tank 22 having a slightly sealed internal space, and an upper portion and a condensation chamber connecting the evaporation tanks 21. The upper communication path 23 of 22 is formed.

蒸發槽21,經由連接到其底部的第1供給路徑P1,儲存著從洗淨裝置10所供給的混合液X1。進一步地,蒸發槽21包含一加熱器24,其位於蒸發槽21的底部附近,以加熱蒸發槽21所儲存的混合液X1。此加熱器24,其控制係用烴類溶劑S及水會蒸發汽化的溫度,加熱混合液X1 。The evaporation tank 21 stores the mixed liquid X1 supplied from the cleaning device 10 via the first supply path P1 connected to the bottom thereof. Further, the evaporation tank 21 includes a heater 24 located near the bottom of the evaporation tank 21 to heat the mixed liquid X1 stored in the evaporation tank 21. The heater 24 is controlled by a hydrocarbon solvent S and a temperature at which water vaporizes and vaporizes, and the mixture X1 is heated.

冷凝槽22的上部充填著在蒸發槽21蒸發汽化的烴類溶劑S及水的氣體,冷凝槽22的下部儲存著烴類溶劑S和水的混合液X2。進一步地,冷凝槽22的上部包含一冷卻器25,用於冷卻蒸發槽21的上部空間。此冷卻器25,其控制係用讓蒸發汽化的烴類溶劑S及水的氣體會液化的溫度,冷卻冷凝槽22的上部空間。連通路徑23,其構成係作為一流動路徑,將在蒸發槽21蒸發汽化的烴類溶劑S及水的氣體,導入冷凝槽22。The upper portion of the condensing tank 22 is filled with a gas of a hydrocarbon solvent S and water evaporated by evaporation in the evaporation tank 21, and a lower portion of the condensing tank 22 stores a mixed liquid X2 of a hydrocarbon solvent S and water. Further, the upper portion of the condensing tank 22 includes a cooler 25 for cooling the upper space of the evaporation tank 21. The cooler 25 is controlled to cool the upper space of the condensing tank 22 by a temperature at which the vaporized hydrocarbon solvent S and the gas of the water are liquefied. The communication path 23 is configured as a flow path for introducing the hydrocarbon solvent S and the water gas evaporated by evaporation in the evaporation tank 21 into the condensation tank 22.

上述構成的真空蒸餾再生裝置20,經由連接到冷凝槽22底部的第2供給路徑,連接到預熱槽30。且,第2供給路徑P2,其係讓用低於烴類溶劑S的引火點之溫度冷卻過的混合液X2流過。The vacuum distillation regeneration device 20 having the above configuration is connected to the preheating tank 30 via a second supply path connected to the bottom of the condensation tank 22. Further, the second supply path P2 is caused to flow through the mixed liquid X2 cooled at a temperature lower than the temperature of the ignition point of the hydrocarbon solvent S.

又,如圖1所示,預熱槽30用作一儲存槽,暫時儲存從真空蒸餾再生裝置20的冷凝槽22經由第2供給路徑P2所供給的混合液X2。進一步地,預熱槽30包含一預熱加熱器31,用預定溫度預熱所儲存的混合液X2。Further, as shown in FIG. 1, the preheating tank 30 serves as a storage tank for temporarily storing the mixed liquid X2 supplied from the condensing tank 22 of the vacuum distillation regeneration apparatus 20 via the second supply path P2. Further, the preheating tank 30 includes a preheating heater 31 for preheating the stored mixed liquid X2 with a predetermined temperature.

此預熱加熱器31,其控制係用在常溫以上、烴類溶劑S不會蒸發汽化的溫度以下之溫度,預熱混合液X2。且,作為混合液X2的溫度,溫度在50度以上80度以下,優選在70度以上80度以下。這是為了縮短後述的加熱裝置60之加熱時間和促進浸透汽化裝置40的浸透汽化。The preheating heater 31 is controlled to preheat the mixed liquid X2 at a temperature equal to or higher than a normal temperature or higher and a temperature at which the hydrocarbon solvent S does not evaporate. Further, as the temperature of the mixed liquid X2, the temperature is 50 degrees or more and 80 degrees or less, preferably 70 degrees or more and 80 degrees or less. This is to shorten the heating time of the heating device 60 to be described later and to promote the permeation vaporization of the permeation vaporization device 40.

以上構成的預熱槽30,經由連接到其底部的第3供給路徑P3,連接到浸透汽化裝置40。如圖1所示,此第3供給路徑P3,係從上游依下列順序設置:一壓送泵浦50,將混合液X2從預熱槽30壓送到浸透汽化裝置40;及一加熱裝置60,加熱流過第3供給路徑P3的混合液X2。The preheating tank 30 configured as above is connected to the permeation vaporization device 40 via the third supply path P3 connected to the bottom thereof. As shown in FIG. 1, the third supply path P3 is disposed from the upstream in the following order: a pressure feed pump 50, pressurizing the mixed liquid X2 from the preheating tank 30 to the permeation vaporization device 40; and a heating device 60 The mixed liquid X2 flowing through the third supply path P3 is heated.

加熱裝置60,例如由包覆第3供給路徑P3外面的加熱器等所構成。此加熱裝置60,其控制係用適於浸透汽化的溫度(例如約120度),加熱朝浸透汽化裝置40流過的混合液X2。The heating device 60 is constituted by, for example, a heater that covers the outer surface of the third supply path P3. The heating device 60 is controlled to heat the mixed liquid X2 flowing through the vaporizing device 40 with a temperature suitable for pervaporation (for example, about 120 degrees).

又,浸透汽化裝置40,係讓已加熱的混合液X2通過後述的分離膜組件412蒸發汽化且分離為烴類溶劑S和水的裝置。如圖1所示,此浸透汽化裝置40,由一讓已加熱的混合液X2流過的裝置主體部41;一一端連接到裝置主體部41且另一端開放到外部的排水路徑42;一經由排水路徑42連接到裝置主體部41的真空泵浦43;一冷卻排水路徑42內部的第1冷卻裝置44;一一端連接到裝置主體部41且另一端連接到第4供給路徑P4的溶劑排出路徑45;及一冷卻溶劑排出路徑45內部的第2冷卻裝置46所構成。Further, the vaporization device 40 is impregnated into a device in which the heated mixed liquid X2 is vaporized by a separation membrane module 412 to be described later and separated into a hydrocarbon solvent S and water. As shown in Fig. 1, the permeation vaporization device 40 is composed of a device main body portion 41 through which the heated mixed liquid X2 flows; a drainage path 42 having one end connected to the device main body portion 41 and the other end open to the outside; The vacuum pump 43 connected to the apparatus main body portion 41 via the drain path 42; the first cooling device 44 inside the cooling drain path 42; the solvent discharge at one end connected to the device main body portion 41 and the other end connected to the fourth supply path P4 The path 45 is formed by a second cooling device 46 inside the cooling solvent discharge path 45.

由圖2所示,裝置主體部41,由一略圓筒狀的外殼411;及一收容保持於外殼411內部的分離膜組件412所構成。外殼411,其係形成讓一連接到第3供給路徑P3且略圓筒狀的上游側連接部411a;一收容保持分離膜組件412且略圓筒狀的主體部411b;及一連接到溶劑排出路徑45且略圓筒狀的下游側連接部411c於同軸上配置的形狀。As shown in Fig. 2, the apparatus main body portion 41 is composed of a substantially cylindrical outer casing 411 and a separation membrane module 412 housed inside the outer casing 411. The outer casing 411 is formed with a substantially cylindrical upstream connection portion 411a connected to the third supply path P3, a substantially cylindrical main body portion 411b for holding the separation membrane module 412, and a solvent discharge The path 45 and the substantially cylindrical downstream side connecting portion 411c are coaxially arranged.

上游側連接部411a及下游側連接部411c,其等係形成為具有略相同內外徑的略圓筒形狀。主體部411b,其係形成為具有比上游側連接部411a及下游側連接部411c的內外徑更大的內外徑之略圓筒形狀。進一步地,側面連接部411d形成於主體部411b的外面,以連接到排水路徑42。The upstream side connecting portion 411a and the downstream side connecting portion 411c are formed in a substantially cylindrical shape having slightly the same inner and outer diameters. The main body portion 411b is formed in a substantially cylindrical shape having an inner and outer diameter larger than the inner and outer diameters of the upstream side connecting portion 411a and the downstream side connecting portion 411c. Further, a side connecting portion 411d is formed outside the main body portion 411b to be connected to the drain path 42.

分離膜組件412,其係作為一分離膜,將混合液X2分離為烴類溶劑S和水。更詳細地,如圖2所示,分離膜組件412,具有與主體部411b的軸向長度略相同的軸向長度,且形成為具有比主體部411b的內徑更小的外型之略圓筒狀。The separation membrane module 412 is used as a separation membrane to separate the mixed liquid X2 into a hydrocarbon solvent S and water. In more detail, as shown in FIG. 2, the separation membrane module 412 has an axial length slightly the same as the axial length of the main body portion 411b, and is formed to have a slightly smaller outer shape than the inner diameter of the main body portion 411b. Cylindrical.

此分離膜組件412,由一略圓筒狀的多孔陶瓷支持體412a及一包覆多孔陶瓷支持體412a外面的沸石分離膜412b所一體形成。且,分離膜組件412,配置成與外殼411內部的主體部411b略同軸。The separation membrane module 412 is integrally formed of a substantially cylindrical porous ceramic support 412a and a zeolite separation membrane 412b covering the outer surface of the porous ceramic support 412a. Further, the separation membrane module 412 is disposed to be slightly coaxial with the main body portion 411b inside the outer casing 411.

上述構成的裝置主體部41,藉由上游側連接部411a的內部空間、分離膜組件412的內徑空間、下游側連接部411c的內部空間,構成一混合液流動路徑L1,讓已加熱的混合液X2及烴類溶劑S流過。The apparatus main body portion 41 having the above configuration constitutes a mixed liquid flow path L1 by the internal space of the upstream side connecting portion 411a, the inner diameter space of the separation membrane module 412, and the inner space of the downstream side connecting portion 411c, so that the heated mixture is mixed. The liquid X2 and the hydrocarbon solvent S flow.

進一步地,裝置主體部41,由外殼411的內面與分離膜組件412的外面之間,構成一蒸汽流動路徑L2,以使後述的透過蒸汽W流動。且,蒸汽流動路徑L2,藉由經由排水路徑42所連接的真空泵浦43,維持略真空狀態。Further, the apparatus main body portion 41 constitutes a steam flow path L2 between the inner surface of the outer casing 411 and the outer surface of the separation membrane module 412 to allow the permeated steam W to be described later to flow. Further, the steam flow path L2 is maintained in a slightly vacuum state by the vacuum pump 43 connected via the drain path 42.

第1冷卻裝置44,由熱交換器等所構成,將從裝置主體部41排出的透過蒸汽W,控制在會液化的溫度。第2冷卻裝置46,由熱交換器等所構成,具有冷卻從裝置主體部41所排出的烴類溶劑S之機能。The first cooling device 44 is composed of a heat exchanger or the like, and the permeated steam W discharged from the apparatus main body portion 41 is controlled to a temperature at which liquefaction is performed. The second cooling device 46 is constituted by a heat exchanger or the like and has a function of cooling the hydrocarbon solvent S discharged from the apparatus main body portion 41.

如圖1所示,上述構成的浸透汽化裝置40,經由連接到溶劑排出路徑45的第4供給路徑P4,連接到洗淨裝置10的第3洗淨槽131上部。此第4供給路徑P4,設有壓送泵浦70,將烴類溶劑S從浸透汽化裝置40壓送到洗淨裝置10。As shown in Fig. 1, the permeation vaporization device 40 having the above configuration is connected to the upper portion of the third cleaning tank 131 of the cleaning device 10 via the fourth supply path P4 connected to the solvent discharge path 45. The fourth supply path P4 is provided with a pressure feed pump 70 for pumping the hydrocarbon solvent S from the permeation vaporization device 40 to the cleaning device 10.

接著說明在上述的溶劑脫水系統1中,從雜質和水和烴類溶劑的混合液,去除雜質及水的溶劑脫水方法。本實施方式中的溶劑脫水方法,由一經由第1供給路徑P1將混合液X1從洗淨裝置10供給到真空蒸餾再生裝置20的蒸餾再生步驟;一加熱已蒸餾再生的混合液X2的加熱步驟;一將已加熱的混合液X2分離為烴類溶劑S和水的分離步驟;及一將分離出的烴類溶劑S回流到洗淨裝置10的步驟而成。Next, a solvent dehydration method for removing impurities and water from a mixed liquid of impurities and water and a hydrocarbon solvent in the above-described solvent dehydration system 1 will be described. The solvent dehydration method in the present embodiment is a distillation regeneration step of supplying the mixed liquid X1 from the cleaning device 10 to the vacuum distillation regeneration device 20 via the first supply path P1, and a heating step of heating the mixed liquid X2 that has been distilled and regenerated. A separation step of separating the heated mixed liquid X2 into a hydrocarbon solvent S and water; and a step of refluxing the separated hydrocarbon solvent S to the cleaning device 10.

經由第1供給路徑P1從洗淨裝置10供給到真空蒸餾再生裝置20的混合液X1,被儲存到真空蒸餾再生裝置20的蒸發槽21時,作為蒸餾再生步驟,真空蒸餾再生裝置20用加熱器24加熱蒸發槽21的混合液X1,使烴類溶劑S及水蒸發汽化。When the mixed liquid X1 supplied from the cleaning device 10 to the vacuum distillation regeneration device 20 via the first supply path P1 is stored in the evaporation tank 21 of the vacuum distillation regeneration device 20, the vacuum distillation regeneration device 20 is used as a distillation regeneration step. 24, the mixed liquid X1 of the evaporation tank 21 is heated to evaporate and vaporize the hydrocarbon solvent S and water.

進一步地,真空蒸餾再生裝置20,藉由冷卻器25冷卻經由連通路徑23導入到冷凝槽22的烴類溶劑S的氣體及水的氣體,使其等相變為烴類溶劑S和水的混合液X2 。這麼一來,真空蒸餾再生裝置20,生成從混合液X1去除雜質的混合液X2,再將混合液X2供給到預熱槽30。此時,真空蒸餾再生裝置20,將冷卻到溫度低於烴類溶劑S的引火點的混合液X2供給到預熱槽30。Further, in the vacuum distillation/regeneration apparatus 20, the gas of the hydrocarbon solvent S introduced into the condensation tank 22 via the communication path 23 and the gas of water are cooled by the cooler 25, and the phase is changed into a mixture of the hydrocarbon solvent S and water. Liquid X2. In this way, the vacuum distillation/regeneration apparatus 20 generates the mixed liquid X2 from which the impurities are removed from the mixed liquid X1, and supplies the mixed liquid X2 to the preheating tank 30. At this time, the vacuum distillation regeneration device 20 supplies the mixed liquid X2 cooled to a temperature lower than the ignition point of the hydrocarbon solvent S to the preheating tank 30.

接著,作為加熱步驟,預熱槽30,用預熱加熱器31預熱混合液X2,例如,加熱到70度以上80度以下的溫度。接著,預熱槽30,經由第3供給路徑P3,將用預熱加熱器31加熱過的混合液X2供給到浸透汽化裝置40。此時,加熱裝置60,將流過第3供給路徑P3的混合液X2,例如,加熱到約120度。Next, as a heating step, the preheating tank 30 preheats the mixed liquid X2 with the preheating heater 31, for example, to a temperature of 70 degrees or more and 80 degrees or less. Next, the preheating tank 30 supplies the mixed liquid X2 heated by the preheating heater 31 to the permeation vaporization device 40 via the third supply path P3. At this time, the heating device 60 heats the mixed liquid X2 flowing through the third supply path P3 to, for example, about 120 degrees.

之後,作為分離步驟,浸透汽化裝置40,讓經由第3供給路徑P3供給到混合液流動路徑L1的混合液X2,通過分離膜組件412分離為烴類溶劑S和水。具體來說,由於蒸汽流動路徑L2是略真空狀態,浸透汽化裝置40經由分離膜組件412蒸發汽化混合液X2中的水。Thereafter, as a separation step, the vaporization device 40 is permeated, and the mixed liquid X2 supplied to the mixed solution flow path L1 via the third supply path P3 is separated into a hydrocarbon solvent S and water by the separation membrane module 412. Specifically, since the steam flow path L2 is in a slightly vacuum state, the saturated vaporization device 40 evaporates the water in the vaporized mixture X2 via the separation membrane module 412.

此時,如圖2所示,分離膜組件412不讓烴類溶劑S透過,只讓透過蒸汽W(水的氣體)透過到蒸汽流動路徑L2。透過蒸汽W,藉由真空泵浦43從側面連接部411d被導出到排水路徑42。接著,浸透汽化裝置40,用第1冷卻裝置44冷卻流過排水路徑42的透過蒸汽W,使其相變為水的液體排出到外部。At this time, as shown in FIG. 2, the separation membrane module 412 does not allow the hydrocarbon solvent S to permeate, and only transmits the vapor W (water gas) to the vapor flow path L2. The steam W is discharged from the side connecting portion 411d to the drain path 42 by the vacuum pump 43. Then, the vaporization device 40 is permeated, and the permeated steam W flowing through the drain path 42 is cooled by the first cooling device 44, and the liquid which is converted into water is discharged to the outside.

另一方面,不能透過分離膜組件412的烴類溶劑S,從下游側連接部411c被排出到溶劑排出路徑45。此時,浸透汽化裝置40,用第2冷卻裝置46冷卻流過溶劑排出路徑45的烴類溶劑S,且將其排出到第4供給路徑P4。此後,已去除雜質及水的烴類溶劑S,經由第4供給路徑P4,回流到第3洗淨部13的第3洗淨槽131。On the other hand, the hydrocarbon solvent S that cannot pass through the separation membrane module 412 is discharged from the downstream side connecting portion 411c to the solvent discharge path 45. At this time, the vaporization device 40 is permeated, and the hydrocarbon solvent S flowing through the solvent discharge path 45 is cooled by the second cooling device 46, and is discharged to the fourth supply path P4. Thereafter, the hydrocarbon solvent S from which the impurities and water have been removed is returned to the third cleaning tank 131 of the third cleaning unit 13 via the fourth supply path P4.

如上所述,將烴類溶劑脫水的溶劑脫水系統1及溶劑脫水方法,可將溫度穩定的混合液X2供給到浸透汽化裝置40,有效率地將混合液X2脫水。具體來說,真空蒸餾再生裝置20,藉由汽化蒸發含有雜質的混合液X1再將其冷卻,生成已去除雜質的混合液X2。As described above, the solvent dehydration system 1 and the solvent dehydration method for dehydrating the hydrocarbon solvent can supply the temperature-stable mixed liquid X2 to the permeation vaporization device 40, and the mixture liquid X2 can be efficiently dehydrated. Specifically, the vacuum distillation regenerating device 20 cools the mixed liquid X1 containing impurities by vaporization to form a mixed liquid X2 from which impurities have been removed.

因此,真空蒸餾再生裝置20,可容易地排出溫度較高且溫度穩定的混合液X2。藉此,溶劑脫水系統1及溶劑脫水方法,可容易且穩定地將溫度較高的混合液X2供給到浸透汽化裝置40。Therefore, the vacuum distillation regeneration device 20 can easily discharge the mixed liquid X2 having a high temperature and a stable temperature. Thereby, the solvent dehydration system 1 and the solvent dehydration method can easily and stably supply the mixed liquid X2 having a relatively high temperature to the permeation vaporization device 40.

進一步地,藉由用加熱裝置60加熱混合液X2,溶劑脫水系統1及溶劑脫水方法,可用較少的熱能將混合液X2加熱到所需的溫度。因此,溶劑脫水系統1及溶劑脫水方法,可將溫度穩定的混合液X2供給到浸透汽化裝置40,有效率地將混合液X2脫水。Further, by heating the mixture X2, the solvent dehydration system 1 and the solvent dehydration method with the heating device 60, the mixture X2 can be heated to a desired temperature with less heat. Therefore, in the solvent dehydration system 1 and the solvent dehydration method, the temperature-stable mixed liquid X2 can be supplied to the permeation vaporization device 40, and the mixed liquid X2 can be efficiently dehydrated.

又,溶劑脫水系統1,包含一預熱槽30,暫時儲存供給到浸透汽化裝置40的混合液X2;及一預熱加熱器31,預熱所儲存的混合液X2;藉由加熱從預熱槽30供給到浸透汽化裝置40的混合液X2,即使在烴類溶劑S的引火點低於真空蒸餾再生裝置20的蒸餾溫度之情況下,也可安全地將溫度穩定的混合液X2供給到浸透汽化裝置40。Further, the solvent dehydration system 1 includes a preheating tank 30 for temporarily storing the mixed liquid X2 supplied to the vaporization device 40; and a preheating heater 31 for preheating the stored mixed liquid X2; and preheating by heating The tank 30 is supplied to the mixed liquid X2 that has permeated the vaporization device 40, and even when the ignition point of the hydrocarbon solvent S is lower than the distillation temperature of the vacuum distillation regeneration device 20, the temperature-stable mixed liquid X2 can be safely supplied to the saturated solution. Vaporization unit 40.

具體來說,在烴類溶劑S的引火點低於蒸餾溫度的情況下,若從真空蒸餾再生裝置20排出高溫的混合液X2,會提高引火的危險性。在這種情況下,真空蒸餾再生裝置20,其構成係讓混合液X2冷卻到低於烴類溶劑S的引火點的溫度再排出。因此,若只用加熱手段加熱混合液X2,恐怕無法將溫度穩定的混合液X2供給到浸透汽化裝置40。Specifically, when the ignition point of the hydrocarbon solvent S is lower than the distillation temperature, if the high-temperature mixed liquid X2 is discharged from the vacuum distillation regeneration device 20, the risk of ignition is increased. In this case, the vacuum distillation regenerating device 20 is configured such that the mixed liquid X2 is cooled to a temperature lower than the ignition point of the hydrocarbon solvent S and discharged. Therefore, if the mixed liquid X2 is heated only by the heating means, the temperature-stable mixed liquid X2 may not be supplied to the pervaporation vaporizer 40.

於是,溶劑脫水系統1藉由包含:一預熱槽30,暫時儲存供給到浸透汽化裝置40的混合液X2;及一預熱加熱器31;預熱所儲存的混合液X2,可將冷卻到低於烴類溶劑S的引火點的溫度之混合液X2,在供給到浸透汽化裝置40之前預熱到預定溫度。因此,相較於直接將混合液X2從真空蒸餾再生裝置20供給到浸透汽化裝置40的情況,溶劑脫水系統1可更安全地將混合液X2供給到浸透汽化裝置40。Thus, the solvent dehydration system 1 temporarily stores the mixed liquid X2 supplied to the pervaporation vaporization device 40 by including a preheating tank 30; and a preheating heater 31; preheating the stored mixed liquid X2, which can be cooled to The mixed liquid X2 which is lower than the temperature of the ignition point of the hydrocarbon solvent S is preheated to a predetermined temperature before being supplied to the pervaporation device 40. Therefore, the solvent dehydration system 1 can supply the mixed liquid X2 to the permeation vaporization device 40 more safely than the case where the mixed liquid X2 is directly supplied from the vacuum distillation regeneration device 20 to the pervaporation vaporization device 40.

進一步地,藉由用加熱裝置60加熱已預熱的混合液X2,溶劑脫水系統1可用較少的熱能將混合液X2加熱到所需的溫度。因此,溶劑脫水系統1可將溫度更穩定的混合液X2供給到浸透汽化裝置40。因此,即使在烴類溶劑S的引火點低於蒸餾溫度的情況下,溶劑脫水系統1也可安全地將溫度穩定的混合液X2供給到浸透汽化裝置40。Further, by heating the preheated mixed liquid X2 with the heating device 60, the solvent dehydration system 1 can heat the mixed liquid X2 to a desired temperature with less heat. Therefore, the solvent dehydration system 1 can supply the temperature-stable mixture X2 to the pervaporation vaporizer 40. Therefore, even in the case where the ignition point of the hydrocarbon solvent S is lower than the distillation temperature, the solvent dehydration system 1 can safely supply the temperature-stable mixed liquid X2 to the pervaporation vaporization device 40.

又,浸透汽化裝置40,包含一用於將混合液X2脫水的分離膜組件412,分離膜組件412由一配置於供給混合液X2的一側之多孔陶瓷支持體412a;及一配置於讓水透過的一側之沸石分離膜412b所構成。藉此,溶劑脫水系統1,藉由溫度穩定的混合液X2和分離膜組件412,可有效率地且穩定地分離出烴類溶劑S和水。Further, the pervaporation vaporizer 40 includes a separation membrane module 412 for dehydrating the mixture X2, the separation membrane module 412 is provided by a porous ceramic support 412a disposed on one side of the supply mixture X2; The zeolite separation membrane 412b on one side is formed. Thereby, the solvent dehydration system 1 can efficiently and stably separate the hydrocarbon solvent S and water by the temperature-stable mixed liquid X2 and the separation membrane module 412.

又,溶劑脫水系統1,包含一洗淨裝置10,用烴類溶劑S去除附著在金屬遮罩M的附著物;一第1供給路徑P1,將用洗淨裝置10生成的混合液X1從洗淨裝置10送到真空蒸餾再生裝置20;及一第4供給路徑P4,將用浸透汽化裝置40脫水的烴類溶劑S回流到洗淨裝置10。藉此,溶劑脫水系統1,可將用浸透汽化裝置40脫水過的烴類溶劑S反覆利用於金屬遮罩M的洗淨。Further, the solvent dehydration system 1 includes a cleaning device 10, and the deposit attached to the metal mask M is removed by the hydrocarbon solvent S. The first supply path P1 is used to wash the mixed liquid X1 produced by the cleaning device 10. The cleaning device 10 is sent to the vacuum distillation regeneration device 20; and a fourth supply path P4, and the hydrocarbon solvent S dehydrated by the pervaporation vaporization device 40 is returned to the cleaning device 10. Thereby, the solvent dehydration system 1 can repeatedly use the hydrocarbon solvent S dehydrated by the pervaporation vaporization apparatus 40 to wash the metal mask M.

在本發明的構成和上述實施方式之間的對應關係中,本發明的水溶性有機溶劑相當於實施方式的烴類溶劑S;以下相同地,有機溶劑和水的混合液相當於混合液X2;供給路徑相當於第2供給路徑P2及第3供給路徑P3;加熱手段相當於加熱裝置60;暫時儲存槽相當於預熱槽30;預熱手段相當於預熱加熱器31;浸透汽化膜組件相當於分離膜組件412;被洗淨物相當於金屬遮罩M;含有雜質及水的有機溶劑相當於混合液X1;送液路徑相當於第1供給路徑P1;回流路徑相當於第4供給路徑P4。但,本發明不僅限定於上述實施方式的構成,可獲得許多實施方式。In the correspondence between the configuration of the present invention and the above embodiment, the water-soluble organic solvent of the present invention corresponds to the hydrocarbon solvent S of the embodiment; in the following, the mixed liquid of the organic solvent and water corresponds to the mixed liquid X2; The supply path corresponds to the second supply path P2 and the third supply path P3; the heating means corresponds to the heating device 60; the temporary storage tank corresponds to the preheating tank 30; the preheating means corresponds to the preheating heater 31; and the saturated vaporization membrane module is equivalent The separation membrane module 412; the object to be washed corresponds to the metal mask M; the organic solvent containing impurities and water corresponds to the mixed liquid X1; the liquid supply path corresponds to the first supply path P1; and the return path corresponds to the fourth supply path P4 . However, the present invention is not limited to the configuration of the above embodiment, and many embodiments are available.

例如,在上述實施方式中,使用烴類溶劑S作為水溶性有機溶劑說明。但,不限定於此,只要是水溶性,也可為適當的有機溶劑。又,使用有機發光二極體的蒸鍍製程使用的金屬遮罩M作為被洗淨物說明。但,不限定於此,只要是使用水溶性的烴類溶劑洗淨的被洗淨物,也可為適當的被洗淨物。For example, in the above embodiment, the hydrocarbon solvent S is used as the water-soluble organic solvent. However, it is not limited thereto, and may be a suitable organic solvent as long as it is water-soluble. Moreover, the metal mask M used for the vapor deposition process of an organic light-emitting diode is demonstrated as a to-be-cleaned material. However, the present invention is not limited thereto, and may be an appropriate material to be washed as long as it is washed with a water-soluble hydrocarbon solvent.

又,由3個洗淨部(第1洗淨部11、第2洗淨部12及第3洗淨部13)構成洗淨裝置10。但,不限定於此,只要是由1個以上的洗淨部構成的洗淨裝置10,也可為適當的構成。例如,也可為用8個洗淨部構成的洗淨裝置。Further, the cleaning device 10 is constituted by three cleaning portions (the first cleaning portion 11, the second cleaning portion 12, and the third cleaning portion 13). However, the present invention is not limited thereto, and may be an appropriate configuration as long as it is a cleaning device 10 composed of one or more cleaning portions. For example, a washing device composed of eight washing portions may be used.

又,除了洗淨裝置10,也可為包含一沖洗用洗淨裝置10洗淨過的被洗淨物之沖洗裝置之溶劑脫水系統。在這種情況下,沖洗被洗淨物的烴類溶劑為非氯代烴溶劑(HFE)等。又,分離膜組件412由多孔陶瓷支持體412a和沸石分離膜412b所構成。但,不限定於此,只要是可藉由浸透汽化將混合液X2分離為烴類溶劑S和水,也可為適當構成的分離膜組件。Further, in addition to the cleaning device 10, it may be a solvent dehydration system that includes a washing device for washing the washed cleaning device 10. In this case, the hydrocarbon solvent for rinsing the object to be washed is a non-chlorinated hydrocarbon solvent (HFE) or the like. Further, the separation membrane module 412 is composed of a porous ceramic support 412a and a zeolite separation membrane 412b. However, the present invention is not limited thereto, and a separation membrane module which is appropriately configured may be used as long as it can separate the mixed liquid X2 into a hydrocarbon solvent S and water by pervaporation.

例如,也可為一多孔陶瓷支持體412a的外面被沸石分離膜412b、二氧化矽分離膜或碳分離膜等的微多孔陶瓷分離膜包覆之分離膜組件412。又,使用多孔陶瓷支持體412a的外面被沸石分離膜412b包覆之分離膜組件412,但不限定於此,也可為多孔陶瓷支持體的內面被沸石分離膜等的微多孔陶瓷分離膜包覆之分離膜組件。For example, the separation membrane module 412 coated with the microporous ceramic separation membrane such as the zeolite separation membrane 412b, the ceria separation membrane or the carbon separation membrane may be used as the outer surface of the porous ceramic support 412a. Further, the separation membrane module 412 whose outer surface of the porous ceramic support 412a is covered with the zeolite separation membrane 412b is not limited thereto, and the inner surface of the porous ceramic support may be a microporous ceramic separation membrane such as a zeolite separation membrane. Coated separation membrane module.

又,溶劑脫水系統1包含一預熱槽30,但不限定於此,例如也可為圖3所示的另一實施方式的溶劑脫水系統1的構成之構成圖,也可不需要預熱槽30,經由第2供給路徑P2及加熱裝置60連接真空蒸餾再生裝置20和浸透汽化裝置40而構成。或,也可進一步地讓圖3的溶劑脫水系統1不需要加熱裝置60而構成。在這種情況下,也可讓真空蒸餾再生裝置20經由第2供給路徑P2,將溫度適於浸透汽化的混合液X2供給到浸透汽化裝置40。Further, the solvent dehydration system 1 includes a preheating tank 30. However, the present invention is not limited thereto. For example, the configuration of the solvent dehydration system 1 of another embodiment shown in Fig. 3 may be employed, and the preheating tank 30 may not be required. The vacuum distillation regeneration device 20 and the pervaporation vaporization device 40 are connected via the second supply path P2 and the heating device 60. Alternatively, the solvent dehydration system 1 of FIG. 3 may be further configured without the need for the heating device 60. In this case, the vacuum distillation regeneration device 20 may supply the mixed liquid X2 having a temperature suitable for pervaporation to the permeation vaporization device 40 via the second supply path P2.

藉此,溶劑脫水系統1及溶劑脫水方法,可使用真空蒸餾再生裝置20作為加熱手段,加熱供給到浸透汽化裝置40的混合液X2。由於溶劑脫水系統1及溶劑脫水方法,可不需要加熱裝置60,故可用簡單的構成有效率地將混合液X2脫水。Thereby, the solvent dehydration system 1 and the solvent dehydration method can be used to heat the supply liquid X2 supplied to the vaporization device 40 by using the vacuum distillation regeneration device 20 as a heating means. Since the solvent dehydration system 1 and the solvent dehydration method do not require the heating device 60, the mixed solution X2 can be efficiently dehydrated with a simple configuration.

1‧‧‧溶劑脫水系統1‧‧‧ solvent dehydration system

10‧‧‧洗淨裝置10‧‧‧cleaning device

11‧‧‧第1洗淨部11‧‧‧1st cleaning department

111‧‧‧第1洗淨槽111‧‧‧1st cleaning tank

112‧‧‧第1儲存槽112‧‧‧1st storage tank

113‧‧‧超音波振動器113‧‧‧Supersonic vibrator

12‧‧‧第2洗淨部12‧‧‧2nd cleaning department

121‧‧‧第2洗淨槽121‧‧‧2nd cleaning tank

122‧‧‧第2儲存槽122‧‧‧2nd storage tank

123‧‧‧超音波振動器123‧‧‧Supersonic vibrator

13‧‧‧第3洗淨部13‧‧‧3rd Washing Department

131‧‧‧第3洗淨槽131‧‧‧3rd cleaning tank

132‧‧‧第3儲存槽132‧‧‧3rd storage tank

133‧‧‧超音波振動器133‧‧‧Ultrasonic vibrator

14‧‧‧第1送液路徑14‧‧‧1st liquid supply path

15‧‧‧第2送液路徑15‧‧‧2nd liquid supply path

20‧‧‧真空蒸餾再生裝置20‧‧‧Vacuum distillation regeneration unit

21‧‧‧蒸發槽21‧‧‧Evaporation tank

22‧‧‧冷凝槽22‧‧‧Condensation tank

23‧‧‧連通路徑23‧‧‧Connected path

24‧‧‧加熱器24‧‧‧heater

25‧‧‧冷卻器25‧‧‧cooler

30‧‧‧預熱槽30‧‧‧Preheating tank

31‧‧‧預熱加熱器31‧‧‧Preheating heater

40‧‧‧浸透汽化裝置40‧‧‧Infiltration vaporization unit

41‧‧‧裝置主體部41‧‧‧The main body of the device

411‧‧‧外殼411‧‧‧ Shell

411a‧‧‧上游側連接部411a‧‧‧ upstream side connection

411b‧‧‧主體部411b‧‧‧ Main Body

411c‧‧‧下游側連接部411c‧‧‧ downstream side connection

411d‧‧‧側面連接部411d‧‧‧Side joints

412‧‧‧分離膜組件412‧‧‧Separation membrane module

412a‧‧‧多孔陶瓷支持體412a‧‧‧Porous ceramic support

412b‧‧‧沸石分離膜412b‧‧‧Zeolite separation membrane

42‧‧‧排水路徑42‧‧‧Drainage path

43‧‧‧真空泵浦43‧‧‧vacuum pump

44‧‧‧第1冷卻裝置44‧‧‧1st cooling unit

45‧‧‧溶劑排出路徑45‧‧‧Solvent discharge path

46‧‧‧第2冷卻裝置46‧‧‧2nd cooling device

50‧‧‧壓送泵浦50‧‧‧Pumping pump

60‧‧‧加熱裝置60‧‧‧ heating device

70‧‧‧壓送泵浦70‧‧‧Pumping pump

L1‧‧‧混合液流動路徑L1‧‧‧ mixture flow path

L2‧‧‧蒸汽流動路徑L2‧‧‧ steam flow path

M‧‧‧金屬遮罩M‧‧‧Metal mask

P1‧‧‧第1供給路徑P1‧‧‧1st supply path

P2‧‧‧第2供給路徑P2‧‧‧2nd supply path

P3‧‧‧第3供給路徑P3‧‧‧3rd supply path

P4‧‧‧第4供給路徑P4‧‧‧4th supply path

S‧‧‧烴類溶劑S‧‧‧ hydrocarbon solvent

W‧‧‧透過蒸汽W‧‧‧through steam

X1‧‧‧混合液X1‧‧‧ mixture

X2‧‧‧混合液X2‧‧‧ mixture

圖1為表示溶劑脫水系統的構成之構成圖。 圖2為表示浸透汽化裝置的裝置主體部的構成之構成圖。 圖3為表示另一實施方式的溶劑脫水系統的構成之構成圖。Fig. 1 is a view showing the configuration of a solvent dehydration system. Fig. 2 is a view showing the configuration of a main body of a device that is saturated with a vaporization device; Fig. 3 is a configuration diagram showing a configuration of a solvent dehydration system according to another embodiment.

Claims (5)

一種溶劑脫水系統,其係包含:  一浸透汽化裝置,將水溶性有機溶劑和水的混合液脫水;  一供給路徑,將該混合液供給到該浸透汽化裝置;及  一加熱手段,將供給到該浸透汽化裝置的該混合液加熱;其中,該溶劑脫水系統更包含一生成該混合液的蒸餾再生裝置,該蒸餾再生裝置經由該供給路徑連接到該浸透汽化裝置。A solvent dehydration system comprising: a pervaporation device for dehydrating a mixture of a water-soluble organic solvent and water; a supply path for supplying the mixture to the pervaporation device; and a heating means for supplying the solution The mixture of the vaporization device is heated; wherein the solvent dehydration system further comprises a distillation regeneration device for generating the mixed liquid, the distillation regeneration device being connected to the pervaporation device via the supply path. 如申請專利範圍第1項所述之溶劑脫水系統,其中該蒸餾再生裝置和該浸透汽化裝置之間係包含:  一暫時儲存槽,暫時儲存供給到該浸透汽化裝置的該混合液;及  一預熱手段;預熱儲存在該暫時儲存槽的混合液;其中,該加熱手段係加熱從該暫時儲存槽供給到該浸透汽化裝置的該混合液。The solvent dehydration system of claim 1, wherein the distillation regeneration device and the permeation vaporization device comprise: a temporary storage tank for temporarily storing the mixed liquid supplied to the pervaporation vaporization device; a heat means; preheating the mixed liquid stored in the temporary storage tank; wherein the heating means heats the mixed liquid supplied from the temporary storage tank to the pervaporation vaporization device. 如申請專利範圍第1項所述之溶劑脫水系統,其中該浸透汽化裝置包含:  一浸透汽化膜組件,其係用於將該混合液脫水;其中,該浸透汽化膜組件係由多孔陶瓷支持體和微多孔陶瓷分離膜的積層體所構成。The solvent dehydration system of claim 1, wherein the pervaporation apparatus comprises: a pervaporation membrane module for dehydrating the mixture; wherein the pervaporation membrane module is a porous ceramic support It is composed of a laminate of a microporous ceramic separation membrane. 如申請專利範圍第1項所述之溶劑脫水系統,包含:  一洗淨裝置,用該有機溶劑去除附著於被洗淨物的附著物;  一送液路徑,將於該洗淨裝置生成的雜質、該水及該有機溶劑之混合液從該洗淨裝置送到該蒸餾再生裝置;及 一回流路徑,將用該浸透汽化裝置脫水過的該有機溶劑回流到該洗淨裝置。The solvent dehydration system according to claim 1, comprising: a cleaning device for removing the adhering matter attached to the object to be washed; and a liquid feeding path for impurities generated in the cleaning device a mixture of the water and the organic solvent is sent from the cleaning device to the distillation regeneration device; and a reflux path is used to reflux the organic solvent dehydrated by the pervaporation device to the cleaning device. 一種溶劑脫水方法,其使用的系統包含:  一浸透汽化裝置,將水溶性有機溶劑和水的混合液脫水;  一供給路徑,將該混合液供給到該浸透汽化裝置;及  一加熱手段,將供給到該浸透汽化裝置的該混合液加熱;其中,該溶劑脫水方法包含:  一蒸餾再生裝置生成該混合液的步驟;  一用加熱手段加熱該混合液的步驟;  一經由該供給路徑將該混合液從該蒸餾再生裝置供給到該浸透汽化裝置的步驟;及  一用該浸透汽化裝置將該混合液脫水的步驟。A solvent dehydration method, the system used comprising: a pervaporation device for dehydrating a mixture of a water-soluble organic solvent and water; a supply path for supplying the mixture to the pervaporation device; and a heating means for supplying Heating the mixture into the vaporization device; wherein the solvent dehydration method comprises: a step of generating a mixture by a distillation regeneration device; a step of heating the mixture by heating; and a mixture of the mixture via the supply path a step of supplying the distillation regeneration device to the pervaporation vaporization device; and a step of dehydrating the mixed liquid with the pervaporation vaporization device.
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