JP4112934B2 - Method and apparatus for recovering liquid medium - Google Patents

Description

【００４３】
【発明の効果】
本発明の方法及び装置は、溶媒を沸騰させずに動作させるので、好ましい稼働状態で溶媒を精製することができる。
【図面の簡単な説明】
【図１】従来の有機溶媒単蒸留装置を示す概略図である。
【図２】従来の有機溶媒分別蒸留装置を示す概略図である。
【図３】本発明による有機溶媒自動精製装置を示す概略図である。
【符号の説明】
１： 蒸発用丸底フラスコ
２： 加温浴
３： 温度計
４： 凝縮用冷却コンデンサー
５： 回収受器
６： 冷媒接続口
７： カラム塔
８： 電磁弁
９： 電磁弁
１０： 液状媒体回収装置
１５： 自動開閉電磁弁
１６： 自動開閉電磁弁
１７： 自動開閉電磁弁
１８： 自動開閉電磁弁
１９： 自動開閉電磁弁
２０： 気化部（加温部、蒸発用丸底フラスコ受器）
２２： 加温部
２４： 液状媒体供給口、回収溶媒供給口
２６： 蒸発用丸底フラスコ受器
２８： 自動開閉電磁弁
３０： 廃液貯留タンク
３２： 枝管
３４： 接続導管
３６： 枝管
４０： 加温浴
４４： 接続導管
５０： 溶媒供給用密閉タンク
５５： 原液溶媒タンク
６０、６４： 接続導管（渡りチューブ配管）
６２、６５、６６： ３方分岐管
７０： 接続導管（供給部）
８０： ニードル開閉弁
８１： 自動開閉電磁弁
９０： 接続導管
１００： 凝縮部（凝縮用冷却コンデンサー、丸底フラスコ受器）
１０２： 凝縮用冷却コンデンサー
１０４： 丸底フラスコ受器
１０６： 精製溶媒貯留タンク
１０８： 枝管
１１０： 枝管
１１２： 接続導管
Ｐ−１： ダイヤフラムポンプ（供給部）
Ｐ−２： 加・減圧デュアルポンプ
Ｐ−３： 温浴循環用ポンプ[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method and apparatus for separating and recovering a liquid medium from a mixture containing a liquid medium, such as a solution containing a solute.
[0002]
[Prior art]
In recent years, interest in environmental issues has increased, and standards such as ISO and PRTR (Pollutant Release and Transfer Register) have become stricter for chemical substances that may be harmful to human health and ecosystems. Yes. In response to such a movement, there is an increasing interest in reusing a used liquid medium in order to reduce the amount of solvent discharged. Recently, as an apparatus for this purpose, an organic solvent distillation apparatus and a solvent regeneration apparatus are used. Various separators are commercially available under the names of automatic solvent recovery devices and the like.
[0003]
However, these apparatuses all use distillation under normal pressure or reduced pressure (a method in which a solvent is heated to the boiling point to produce saturated vapor, and this saturated vapor is separated) as the principle of medium separation. The figures are shown in FIGS. FIG. 1 shows an organic solvent simple distillation apparatus that is widely used. The boiled solvent vapor is led to a condensing part (condensing cooling condenser 4), where it is condensed to separate and purify the solvent. The distillation apparatus of FIG. 2 is an apparatus for separating and purifying a mixed solvent in which two or more kinds of solvents are mixed into a single component solvent, and the evaporation section of this apparatus is filled with the solvent, and the evaporation bottom of the evaporation section The flask 1 is connected to a vertically extending fraction (column tower 7), and a condensing part (condensing cooling condenser 4) is connected to the upper part of the column. This branch pipe is further devised so that a part of the condensate is refluxed to the upper part of the fractionation column tower 7 at the upper part, and the recovery and the reflux are controlled by electromagnetic valves 8 and 9. Thus, the solvent can be fractionally distilled. In short, it is used as an apparatus for purifying a mixed solvent while boiling an organic solvent and appropriately switching between reflux and fractionation.
[0004]
In Japanese Patent Application No. 4-86978, high-purity n-butanol and water from a used waste liquid consisting of n-butanol, butyl acetate, water, 2-butoxyethanol, 2-hexyloxyethanol, and an aqueous phase are used. A method is described in which the solvent phase is precipitated and separated and recovered by repeated rectification under reduced pressure. However, this method also rectifies by boiling the solvent.
[0005]
However, in these apparatuses, in principle, the organic solvent is boiled and “distilled” under normal pressure or reduced pressure, and as a disadvantage of these apparatuses, (1) the force of solvent vapor pressure is used. Therefore, the solvent needs to be heated to the boiling point or higher, and therefore the heating bath 40 of the evaporation round bottom flask receiver 26 needs to be heated higher than the boiling point of the solvent. Therefore, in an organic solvent having a low flash point, From the viewpoint of safe operation, human attention is always indispensable. Furthermore, (2) In conventional equipment that is not a circulation system, due to structural limitations during continuous operation, additional solvents and removal of purified solvents are required. In addition, there are many problems to be solved such as a complicated mechanism on the apparatus for automating the discharge of the concentrated mother liquor, and (3) solving the complexity of the apparatus and the complexity of operation.
[0006]
[Patent Document 1]
Japanese Patent No. 4-86978
[0007]
[Problem to be Solved by the Invention]
An object of the present invention is to solve the above-mentioned drawbacks of the conventional apparatus, and in particular to provide a novel method and apparatus for “separation and purification” without requiring boiling of the solvent.
[0008]
The present invention so Forcibly brings gas into contact with the liquid medium, vaporizes the liquid medium, and condenses the vaporized medium Is preferable .
[0009]
The present invention so Uses the gas separated by condensing the medium as the gas that is forced to contact the liquid medium Is preferable .
[0010]
The present invention so When vaporizing a liquid medium, the temperature of the liquid medium is vaporized at a temperature below the boiling point. Is preferable .
[0011]
The present invention so Includes a vaporization unit that forces gas to contact the liquid medium and vaporizes the medium, and a condensing unit that condenses the medium vaporized in the vaporization unit. Is preferable .
[0012]
The present invention so Is separated by forcing gas into contact with the liquid medium to vaporize the liquid medium, a condensing part for condensing the medium vaporized in the vaporizing part, and condensing in the condensing part A separation gas supply unit that supplies the separation gas to the vaporization unit as a gas that is forced to contact the liquid medium. Is preferable .
[0013]
BEST MODE FOR CARRYING OUT THE INVENTION
First, the meaning of the terms in this specification will be described. “Liquid medium” is not particularly limited as long as it is in the state of being subjected to treatment with the method or apparatus according to the present invention, and may be one kind of medium or a mixture of two or more kinds, or an organic solvent. It may be an inorganic solvent, and may be a polar solvent or a nonpolar solvent. However, it is typically a medium that is liquid at room temperature and pressure. As the liquid medium, for example, a low boiling point medium having a boiling point of 50 ° C. or less, for example, ether, methylene chloride, pentane, a medium boiling point medium having a boiling point of 50 to 100 ° C., for example, THF, ethyl acetate, chloroform, acetone, hexane, ethanol, or Examples thereof include alcohols such as methanol and high-boiling media having a boiling point of 100 ° C. or higher, such as benzene, toluene, DMF, DMSO, and acetonitrile.
[0014]
Further, the liquid medium to be treated may be in a homogeneous material system such as a solution, a suspension, an emulsion, or the like, or in a heterogeneous material system. Specifically, the state after using a liquid medium as an extractant, a cleaning agent, an eluent, a developing agent, an absorbent, etc. can be mentioned. Examples thereof include separation and purification of extracts such as herbal medicines, and column chromatography eluents or washing liquid regeneration treatments.
[0015]
The “gas” is not particularly limited as long as it is inert to the liquid medium to be treated and can maintain a gaseous state even when cooled with a refrigerant. It should be noted that an appropriate gas is selected according to conditions (for example, vaporization conditions and condensation conditions) determined in consideration of the liquid medium subjected to the treatment. Specific examples include air, nitrogen, helium, and argon, but air is preferable from the viewpoint of cost.
[0016]
The “gas separated by condensing the medium” is a gas that has passed through the condensing part, and the medium in which the liquid medium is vaporized is mixed with the gas. However, when the medium passes through the condensing part, the medium is condensed. Thus, it is a gas that does not contain a medium because it is a liquid medium and separated from the gas. Therefore, the partial pressure of the medium is very small, and the medium is easily vaporized when the gas and the medium are forcibly brought into contact with each other. However, depending on the condensation conditions, the gas may contain some medium.
[0017]
“Forced contact” means that the gas-liquid contact is mechanically and artificially changed by changing the gas into an air current using a pump, etc., and blowing this air current onto a liquid such as a medium or bubbling the liquid. By doing this, the boundary film portion formed at the interface between the liquid and the gas is forced to be blown away by bringing the air current into contact therewith, and the boundary film portion is constantly updated.
[0018]
Next, various conditions for recovering the liquid medium in the method and apparatus of the present invention will be described. First, regarding forced contact, for example, a contact method such as countercurrent, flat flow, crossing, spraying, or the like can be used. In the case of countercurrent contact, the mixture is supplied from the top to the wall, and the gas is passed from the bottom to the top. Double spiral pipe, heated by the outer pipe, wetted into the inner pipe. It is preferable to flow. Moreover, it can be made to contact by passing or spraying gas on the surface of a mixture. Furthermore, a gas can be passed through the mixture, for example bubbling. On the other hand, the contact efficiency can be increased by spraying, but in this case, it is preferable to spray fine particle droplets that do not become mist.
[0019]
Regarding the heating, it is preferable that the temperature of the liquid medium is vaporized at a temperature equal to or lower than the boiling point. For example, for an organic solvent having a high boiling point and a medium boiling point, the bath temperature may be adjusted to a temperature lower by 10 to 20 ° C. than the boiling point. For low-boiling organic solvents, it is preferable to adjust the bath temperature 5-10 ° C. below the boiling point. However, you may vaporize at the temperature more than a boiling point.
[0020]
Next, regarding the condensing condition, it is sufficient if the vaporized medium is in a temperature condition that becomes a liquid. However, in order to increase the efficiency, it is preferable to set the condensing temperature of the medium to a lower temperature.
In the case of a low boiling point medium, 0 to -40 ° C is preferable, and -10 to -30 ° C is more preferable. In the case of a medium boiling point medium, 10 to -30 ° C is preferable, and 0 to -20 ° C is more preferable.
In the case of a high boiling point medium, 20 to -20 ° C is preferable, and 10 to -10 ° C is more preferable.
[0021]
In addition, as a suitable thing of this invention, the aspect which circulates gas by making it a closed system can be mentioned. By adopting such an aspect, in addition to being environmentally safe without the risk of the medium being diffused to the outside, even when condensation in the condensing part is insufficient, the gas is high due to reflux. The recovery rate can be maintained.
[0022]
A liquid medium recovery apparatus according to a preferred embodiment of the present invention is shown in FIG.
The liquid medium recovery apparatus 10 includes a heating unit 22, a condenser cooling condenser 102, and connection conduits 70, 60, and 64 that connect the upper and lower parts thereof, and an annular circulation that is closed by the liquid medium recovery apparatus 10. Build the system. A diaphragm pump P-1 made of fluororesin for gas circulation is attached between the connecting conduits 60 and 64. By forcibly circulating the gas contained in the annular circulation system by the diaphragm pump P-1, the liquid medium injected into the vaporization unit 20 from the liquid medium supply port 24 is vaporized and purified and liquefied and collected by the condensing unit 100. Is done.
[0023]
The material used for the apparatus of the present invention is not particularly limited as long as it is a material that is impermeable to gases and liquids and has chemical resistance. Examples of materials include inorganic materials such as carbon materials, glass / enamels, stainless steel, ceramics; polyethylene, polypropylene, tetrafluoroethylene resin, trifluorochloroethylene resin, vinylidene fluoride resin, fluorinated ethylenepropylene resin Organic materials such as perfluoroalkoxy resins, unsaturated polyesters, epoxy resins, vinyl ester resins, furan resins, fluororesins; new metals such as titanium, noble metals such as Pt, Al-Mg alloys, Cu alloys (for example, Metal materials such as Cu—Sn alloys, Su—Zn alloys, Cu—AL alloys, Cu—Ni alloys), Ni alloys (eg, Ni—Cu alloys, Ni—Mo alloys, Ni—Cr alloys); or composite materials Or a material coated with a corrosion-resistant material. Glass, fluororesin and stainless steel are preferred.
[0024]
The pump used for gas circulation should just be a pump provided with chemical resistance, and the inside is a diaphragm pump P-1 made of fluororesin. By using the diaphragm pump P-1 under conditions where steam mist is not generated, gas can be circulated gently in the circulation system.
Moreover, as the gas transfer capability of the diaphragm pump P-1, it is necessary to have the capability to circulate a gas having a volume in the range of 0.1 to 10 times the total internal volume of the liquid medium (organic solvent) automatic purifier per minute. However, it is preferable to use a diaphragm pump capable of circulating a volume of gas in the range of 0.3 to 3 times per minute. For example, if the total internal volume of the organic solvent automatic refining apparatus is 3 to 4 L, a fluororesin diaphragm pump having an exhaust capacity of 15 to 1 L / min can be used. A diaphragm pump with an amount of 8 to 3 L / min may be used.
[0025]
The organic solvent is dropped from a recovery solvent supply port 24 of a fluororesin conduit at the top of the vaporization unit 20 including the heating unit 22 and the evaporation round bottom flask receiver 26, and a part of the organic solvent is added to the heating unit 22. It flows down the inner wall and reaches the round bottom flask receiver 26 for evaporation. The organic solvent dropped and injected is heated and vaporized in the vaporization unit 20 including the heating unit 22 and the round bottom flask receiver 26 for evaporation.
[0026]
A connecting pipe 60 made of fluororesin is inserted into one branch pipe 36 attached between the heating unit 22 and the round bottom flask receiver 26 for evaporation. The distance between the bottom of the evaporating round bottom flask receiver 26 and the tip of the connecting conduit 60 is adjusted depending on the type of organic solvent. Preferably, the tip of the connecting conduit 60 is the evaporating round bottom flask receiver 26. The connecting conduit 60 is fixed so as to be approximately 4 to 8 cm away from the bottom. The other end of the connection conduit 60 is connected to the diaphragm pump P-1. The vaporization of the organic solvent is performed by blowing a gas supplied from the other end of the connection conduit 60 to the liquid level of the evaporation round bottom flask receiver 26 by the diaphragm pump P-1. Further, the tip of the connection conduit 60 may be positioned so as to come into contact with the organic solvent accumulated in the evaporation round bottom flask receiver 26 and bubbled. Further, by supplying gas to the round bottom flask receiver 26 for evaporation, the organic solvent dripped and injected from the recovery solvent supply port 24 is countercurrently raised from the bottom to the top inside the heating unit 22. Air current is generated.
[0027]
A connecting pipe 34 made of a fluororesin is inserted into another branch pipe 32 between the heating unit 22 and the round bottom flask receiver 26 for evaporation. The connection conduit 34 is fixed so that one end of the connection conduit 34 is about 2 cm away from the bottom of the evaporation round bottom flask receiver 26. Further, the other end of the connection conduit 34 is connected to the automatic opening / closing electromagnetic valve 28, and the outlet of the automatic opening / closing electromagnetic valve 28 is connected to the waste liquid storage tank 30 via the connection conduit 44. Thereby, the residual liquid accumulated in the evaporation round bottom flask receiver 26 can be moved from the evaporation round bottom flask receiver 26 to the waste liquid storage tank 30.
[0028]
The recovered organic solvent is dropped from the recovered solvent supply port 24 of the fluororesin conduit at the upper portion of the vaporizing unit 20, and the dropping speed is adjusted by the needle opening / closing valve 80. One end of a conduit 72 is connected to the upper part of the solvent supply sealed tank 50. The other end of the conduit 72 is connected to one end of the three-way branch pipe 62, and the other two ends of the three-way branch pipe 62 are connected so that the conduit 74 circulates. The conduit 74 is connected to the automatic opening / closing solenoid valve 16, the three-way branch pipe 66, the pressure / decompression dual pump P-2, the three-way branch pipe 65, and the automatic opening / closing solenoid valve 15 in this order. Further, the automatic opening / closing electromagnetic valve 17 is connected to the three-way branch pipe 66, and the automatic opening / closing electromagnetic valve 18 is connected to the three-way branch pipe 65.
One end of a conduit 76 is connected to the solvent supply sealed tank 50. The other end of the conduit 76 is connected to the recovered solvent supply port 24 via a needle opening / closing valve 80 and an automatic opening / closing electromagnetic valve 81.
The solvent supply airtight tank 50 is controlled by controlling the activation of the pressure-reducing dual pump P-2 and the opening / closing operations of the automatic opening / closing solenoid valves 15, 16, 17, 18, 19, 81, etc. at preprogrammed timing. It can be in a pressurized state or a reduced pressure state.
Supply of the recovered organic solvent to the vaporization unit 20 is performed as follows.
First, the automatic open / close solenoid valve 19 is opened and the automatic open / close solenoid valve 81 is closed, and the solvent supply sealed tank 50 is brought into a reduced pressure state by using a pressure / decompression dual pump P-2. The stock solution solvent tank 55 is moved to the solvent supply sealed tank 50. Thereafter, the automatic opening / closing solenoid valves 15, 17, 19 are closed and the automatic opening / closing solenoid valves 16, 18, 81 are opened, and the solvent supply sealed tank 50 is weakly pressurized using the pressure-depressurization dual pump P-2. By doing so, the recovered organic solvent is moved from the solvent supply sealed tank 50 to the heating unit 22. Using the pressure / decompression dual pump P-2, the automatic opening / closing solenoid valves 15, 16, 17, 18, 19, 81, etc. are closed. Can control the pressurization / depressurization state of the solvent supply airtight tank 50 by operating the automatic opening / closing electromagnetic valves 16, 18, 81 at a preprogrammed timing.
[0029]
The control of the pressurizing / depressurizing dual pump P-2, the automatic opening / closing electromagnetic valve 28, and the like can be performed at set time intervals by a device such as a timer. This time interval can be appropriately selected according to a predetermined condition, for example, an increasing amount of the residual solution accumulated in the evaporation round bottom flask receiver 26. For example, by monitoring the liquid level of the recovered organic solvent in the solvent supply sealed tank 50, the residual solution of the evaporation round bottom flask receiver 26 is removed from the outside by using the pressure-reducing dual pump P-2. It can be automatically moved to the waste liquid storage tank 30.
[0030]
A heating bath 40 is provided below the evaporation round bottom flask receiver 26 of the vaporization unit 20, and the evaporation round bottom flask receiver 26 is immersed in the heating bath 40 and warmed. A heating unit 22 is connected to the heating bath 40 by a conduit 90. A warm bath circulation pump P-3 is attached to the conduit 90, and the warm bath liquid enclosed in the warm bath 40, the conduit 90, and the warming section 22 is circulated by the warm bath circulation pump P-3 to be heated. The warm bath 40 and the heating unit 22 can be heated.
[0031]
The heating of the evaporation round bottom flask receiver 26 and the heating unit 22 is performed at a temperature equal to or lower than the boiling point of the organic solvent dropped and injected from the recovered solvent supply port 24. Warm to a temperature lower by about 10 to 20 ° C. than the boiling point of the solvent, and in the case of an organic solvent having a low boiling point, the temperature should be about 5 to 10 ° C. lower than the boiling point of the individual solvent. It is preferable to set them individually in consideration of the vaporization characteristics. Therefore, the temperature of the warming bath 40 is desirably set lower than the boiling point of the organic solvent to be purified, and is preferably kept 5 to 20 ° C. lower than the boiling point of the organic solvent.
[0032]
As another aspect of the vaporization unit 20 of the present invention, the evaporation function in the heating unit 22 may not necessarily be provided. For example, only one or a plurality of gas blowing parts such as the evaporation round bottom flask receiver 26 are prepared, and the gas blowing parts are supplied from the gas circulation diaphragm pump P-1 while appropriately heating these gas blowing parts. A gas may be blown to each of the gas blowing portions to vaporize the organic solvent, and these gases may be collected and guided to the cooling condenser 102 for condensation.
[0033]
At this time, in addition to the evaporation round bottom flask receiver 26 described above, a plurality of test tubes are prepared in a sealed box, and a solvent is stored in these test tubes to blow a gas. In particular, there are no particular restrictions on the form of spraying, as long as the gas can be forcibly brought into contact with the organic solvent.
[0034]
When the organic solvent is dropped and injected from the upper recovery solvent supply port 24 of the heating unit 22, it is injected using a heating / depressurizing dual pump P-2. The amount of the recovered solvent injected by the pressure-reducing dual pump P-2 needs to be adjusted depending on the degree of evaporation depending on the type of the recovered organic solvent. Furthermore, the adjustment can be more precisely controlled by using a fluorine resin needle opening / closing valve 80 attached to the organic solvent automatic purifier. The flow rate at the time of dropping injection is preferably adjusted by opening and closing the needle opening / closing valve 80 by referring to the numerical value examined in advance according to the type of the recovered organic solvent. It is preferable that a small amount of the obtained solvent is accumulated in the evaporation round bottom flask receiver 26.
[0035]
The gas evaporated in the evaporation round bottom flask receiver 26 is moved to the heating unit 22, and the organic solvent that is further evaporated in the heating unit 22 is taken into the gas. The heating unit 22 of the vaporization unit 20 and the condensing cooling condenser 102 of the condensing unit 100 are connected by a connection conduit 70. The vaporized vapor vaporized in the vaporization unit 20 moves slowly to the condensation unit 100. The refrigerant flows through the cooling pipe of the condenser cooling condenser 102 of the condensing unit 100, and the vaporized vapor is condensed and liquefied in the condenser cooling condenser 102. The organic solvent condensed almost completely in the condenser cooling condenser 102 is collected in the round bottom flask receiver 104. The refrigerant vapor can be condensed by flowing a refrigerant in the range of 0 to −35 ° C. through the cooling pipe of the condenser for condensing 102, but it is more preferable to flow a refrigerant at −10 ° C. or lower.
[0036]
A fluororesin connection pipe 64 connected to the diaphragm pump P-1 is connected to one branch pipe 108 between the cooling condenser 102 for condensing and the round bottom flask receiver 104. The connecting pipe 60 made of fluororesin connected to the diaphragm pump P-1 is connected to one branch pipe 36 between the heating unit 22 and the round bottom flask receiver 26 for evaporation. In this way, the gas pushed out from the connection conduit 60 returns to the diaphragm pump P-1 from the connection conduit 64 via the heating unit 22, the connection conduit 70, and the condenser cooling condenser 102, thereby closing the system. Circulate inside.
[0037]
A connecting conduit 112 is connected to the other branch 110 between the condensing cooling condenser 102 and the round bottom flask receiver 104, and the connecting conduit 112 is led to the purified solvent storage tank 106. The purified solvent collected in the round bottom flask receiver 104 at the lower part of the condensing unit 100 is automatically moved to the purified solvent storage tank 106 by fixing the height of the connecting conduit 112 appropriately.
[0038]
In addition, it is good also as a structure which provides a three-way branch pipe in the middle of the connection conduit | pipe 64, and connects a further pressurization pump and an automatic on-off valve to the remaining edge part of a three-way branch pipe. The automatic open / close valve connected to this pressurizing pump P-4 (not shown) is opened and pressurized by the pressurizing pump P-4, and purified from the round bottom flask receiver 104 to the purifying solvent storage tank 106. The solvent can be moved automatically. Further, the residue accumulated in the evaporation round bottom flask receiver 26 can be moved to the external waste liquid storage tank 30.
[0039]
In the above-described example, the equipment such as the round bottom flask receiver 26 for evaporation in which the dropped organic solvent and the residual solution are stored and the round bottom flask receiver 104 in which the purified solvent is stored are made of glass. However, other materials, for example, a tool made of the material used in the above-described apparatus of the present invention may be used, and a tool that takes into consideration the operating temperature range, chemical resistance, etc. determined according to the type of solvent used is used. be able to.
[0040]
【Example】
Hereinafter, the present invention will be described in more detail based on examples. These examples do not limit the invention in any way.
[0041]
Example 1
In the liquid medium recovery apparatus 10 of the present invention, 100 mL of an ethanol-containing material used as a chromatographic eluent is introduced into a solvent supply sealed tank 50, and a recovery solvent supply port 24 is added using a pressure-reduction dual pump P-2. The recovered organic solvent was dropped into the closed system at an injection flow rate of 34 mL / min. Adjusting the diaphragm pump P-1 so that the gas flow rate is 6 L / min, the tip of the conduit 60 fixed by the branch pipe 36 via the conduit 60 (outer diameter 6 mm, inner diameter 4 mm) is 1 L capacity. The conduit 60 was placed 6 cm away from the bottom of the evaporating round bottom flask receiver 26. In this way, an inclined ring with a depth of about 2 to 4 mm is formed on the liquid surface of the recovered organic solvent collected in the round-bottom flask receiver 26 for evaporation about 3 to 4 cm. Gas was blown over the recovered organic solvent. The gas blown to the bottom of the evaporation round bottom flask receiver 26 moves to the top of the flask together with the vaporized ethanol and reaches the heating unit 22. The heating unit 22 includes a straight tubular evaporation unit (inner diameter 60 mm, length of about 200 mm) and a snake tube made of a tube having an outer diameter of 8 mm disposed therein, and the helical diameter of the snake tube is 55 mm in outer diameter. . A warm bath solution is supplied from the warm bath 40 into the tube of the serpentine tube by a warm bath circulation pump P-3, and the warm bath solution is circulated between the warm bath 40 and the warming portion 22 including the serpent tube, and the warm bath 40 and the warm bath are heated. Portion 22 was kept at 65 ° C. Thus, the recovery solvent dropped from the recovery solvent supply port 24 moves downward along the outer surface of the serpentine tube and the inner wall surface of the straight tubular evaporation unit inside the heating unit 22, and moves upward from the lower part of the heating unit. Part of the gas was vaporized. Ethanol vaporized in both the evaporating round bottom flask receiver and the heating unit 22 gradually reaches the condensing cooling condenser 102 via the connecting conduit 70, where it is cooled to condense the ethanol into a liquid state. The volume gradually accumulated in a round bottom flask receiver 104. Under the above conditions, almost the whole amount (> 99%) of ethanol was recovered in the round bottom flask receiver 104 at a rate of about 8.5 mL / min.
Examples 2-5
The same procedure as in Example 1 was performed except that the type of the recovery solvent, the heating bath, the recovery solvent injection flow rate, and the pump P-1 flow rate were changed to Table 1. The obtained results are shown in Table 1.
[0042]
[Table 1]

[0043]
【The invention's effect】
Since the method and apparatus of the present invention operate without boiling the solvent, the solvent can be purified in a preferable operating state.
[Brief description of the drawings]
FIG. 1 is a schematic view showing a conventional organic solvent single distillation apparatus.
FIG. 2 is a schematic view showing a conventional organic solvent fractional distillation apparatus.
FIG. 3 is a schematic view showing an organic solvent automatic purification apparatus according to the present invention.
[Explanation of symbols]
1: Round bottom flask for evaporation
2: Heating bath
3: Thermometer
4: Cooling condenser for condensation
5: Collection receiver
6: Refrigerant connection port
7: Column tower
8: Solenoid valve
9: Solenoid valve
10: Liquid medium recovery device
15: Automatic open / close solenoid valve
16: Automatic open / close solenoid valve
17: Automatic open / close solenoid valve
18: Automatic open / close solenoid valve
19: Automatic open / close solenoid valve
20: Vaporization part (heating part, round bottom flask receiver for evaporation)
22: Heating part
24: Liquid medium supply port, recovery solvent supply port
26: Round bottom flask receiver for evaporation
28: Automatic open / close solenoid valve
30: Waste liquid storage tank
32: Branch pipe
34: Connection conduit
36: Branch pipe
40: Heating bath
44: Connection conduit
50: Sealed tank for solvent supply
55: Stock solvent tank
60, 64: Connection conduit (transition tube piping)
62, 65, 66: 3-way branch pipe
70: Connection conduit (supply section)
80: Needle on / off valve
81: Automatic open / close solenoid valve
90: Connecting conduit
100: Condensing part (condensing cooling condenser, round bottom flask receiver)
102: Cooling condenser for condensation
104: Round bottom flask receiver
106: Purified solvent storage tank
108: Branch pipe
110: Branch pipe
112: Connecting conduit
P-1: Diaphragm pump (supply unit)
P-2: Pressure / pressure reduction dual pump
P-3: Hot bath circulation pump

Claims (5)

A method of recovering a liquid medium by evaporating and condensing the liquid medium from a mixture containing the liquid medium,
In means to vaporize, to a mixture containing a liquid medium which is continuously instillation, the gas forcibly the contacted countercurrently to vaporize the liquid medium, and moved to a means for condensing the vaporized said medium,
A gas separated by condensing the medium is used as the gas forced to contact the liquid medium.
A method for recovering a liquid medium. As a means for vaporization, a double spiral tube having a straight tube evaporator and a serpentine tube disposed therein is used, and forced contact by countercurrent between the mixture and gas causes the mixture to flow outside the serpentine tube. 2. The method for recovering a liquid medium according to claim 1, wherein the liquid medium is moved downward along the surface and the inner wall surface of the straight tubular evaporator, and is brought into contact with the gas flowing from the lower part to the upper part of the double spiral pipe. . The recovery of the liquid medium is carried out by closed circulation under reduced pressure, or when the liquid medium is vaporized, the temperature of the liquid medium is vaporized at a temperature below the boiling point, or
  The method for recovering a liquid medium according to claim 1, wherein the liquid medium is vaporized at a temperature equal to or lower than a boiling point when the liquid medium is vaporized at a reduced pressure or when the liquid medium is vaporized. A liquid medium recovery device for vaporizing and condensing and separating a liquid medium from a mixture containing the liquid medium,
In the vaporizing means, a vaporizing unit for vaporizing the liquid medium by forcibly contacting the gas countercurrently with the mixture containing the liquid medium continuously dropped and injected ;
A condensing part for condensing the medium vaporized in the vaporizing part;
A separation gas supply unit that supplies the vaporization unit as a gas that forces the separation gas separated by being condensed in the condensation unit to come into contact with the liquid medium;
Only including,
Force the gas counter-currently to vaporize the liquid medium and move it to a means for condensing the vaporized medium.
The including liquid medium collecting device. As a means for vaporization, a double spiral tube having a straight tube evaporator and a serpentine tube disposed therein is used, and forced contact by countercurrent between the mixture and gas causes the mixture to flow outside the serpentine tube. The liquid medium recovery apparatus according to claim 4, wherein the liquid medium recovery apparatus is moved by moving downward along a surface and an inner wall surface of the straight tubular evaporator and contacting with the gas flowing from the lower part to the upper part of the double spiral pipe.

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