WO2012115081A1 - Dispositif de déshydratation de solvant organique - Google Patents
Dispositif de déshydratation de solvant organique Download PDFInfo
- Publication number
- WO2012115081A1 WO2012115081A1 PCT/JP2012/054058 JP2012054058W WO2012115081A1 WO 2012115081 A1 WO2012115081 A1 WO 2012115081A1 JP 2012054058 W JP2012054058 W JP 2012054058W WO 2012115081 A1 WO2012115081 A1 WO 2012115081A1
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- organic solvent
- dehydrating
- dehydration
- solvent
- tank
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/08—Thickening liquid suspensions by filtration
- B01D17/10—Thickening liquid suspensions by filtration with stationary filtering elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/34—Regenerating or reactivating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J39/00—Cation exchange; Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
- B01J39/08—Use of material as cation exchangers; Treatment of material for improving the cation exchange properties
- B01J39/16—Organic material
- B01J39/18—Macromolecular compounds
- B01J39/20—Macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
- B01D15/36—Selective adsorption, e.g. chromatography characterised by the separation mechanism involving ionic interaction
- B01D15/361—Ion-exchange
- B01D15/362—Cation-exchange
Definitions
- the present invention relates to an apparatus for dehydrating water from an organic solvent, and more particularly to an organic solvent dehydrating apparatus used for dehydrating an organic solvent recovered from an organic solvent-containing gas generated from various factories or research facilities using a solvent recovery apparatus. .
- Patent Document 2 a dehydration step of adsorbing moisture contained in an organic solvent to the dehydrating material by passing the organic solvent through the dehydrating material packed in a dehydrating tank (adsorption tower). And an organic solvent dehydration apparatus using a cation exchange resin as a dehydrating material, and a drying step of drying moisture adsorbed on the dehydrating material by passing an inert gas or air through the dehydrating material. Yes.
- the dehydrating material when an ion exchange resin or the like is used as the dehydrating material, if the drying speed is increased when the dehydrating material is dried after the dehydrating step, the dehydrating material is destroyed due to a difference in water content between the inner and outer layers of the dehydrating material. As a result, clogging occurs in the filter provided in the dewatering tank due to debris of the dehydrating material, which may reduce the dewatering ability of the organic solvent dewatering apparatus.
- the present invention has been made against the background of the problems of the prior art, and it is an object of the present invention to provide an organic solvent dehydrating apparatus having a configuration that does not reduce the dehydrating ability of the organic solvent dehydrating apparatus.
- the base structure of the cation exchange resin is at least one selected from the group consisting of an acrylic acid polymer, a methacrylic acid polymer, and a styrene-divinylbenzene copolymer, Carboxylic acid Ca group or sulfonic acid Na group is provided.
- a dehydrating tank filled with the dehydrating material, an organic solvent introduction path for introducing the organic solvent to be treated into the dehydrating tank, and an inert gas for introducing an inert gas into the dehydrating tank
- the apparatus further includes a washing water introduction path for introducing washing water into the dehydration tank and a washing water discharge path for discharging the washing water from the dehydration tank.
- the washing water introduction path has a washing water circulation path for introducing the washing water discharged to the washing water discharge path into the washing water introduction path.
- the dehydration tank includes a first dehydration tank and a second dehydration tank, and when the drying air is introduced into the first dehydration tank through the dry air introduction path, When the organic solvent to be treated is introduced into the second dehydration tank through the organic solvent introduction path, and the drying air is introduced into the second dehydration tank through the dry air introduction path, the organic solvent introduction path to be treated is introduced.
- the organic solvent to be treated is continuously introduced into the dehydrating material and brought into contact with the dehydrating material, so that the moisture contained in the organic solvent to be treated is reduced. Dehydration removal is possible.
- organic solvent dehydrating apparatus based on the present invention, it is possible to provide an organic solvent dehydrating apparatus having a configuration that does not reduce the dehydrating ability.
- An organic solvent dehydrating apparatus based on the present invention includes a dehydration process facility for allowing an organic solvent containing water to flow through a dehydrating material filled in a dehydrating tank and adsorbing moisture to the dehydrating material, and drying air to the dehydrating material. It is preferable that the organic solvent dehydrator is provided with a drying process facility for passing the water adsorbed on the dehydrating material through the flow and alternately performing the process. This is because the processing can be continuously performed by adopting such a structure.
- the purge water discharged from the water or dry air discharge line 26 contains an organic solvent and may be accumulated and incinerated. However, the damper 27 is opened and the return line 28 is covered. It is preferable to return to the treated organic solvent tank 2. This is because the number of steps can be omitted and this method is efficient.
- the damper 13 is closed and the damper 22 is opened, and the dry air is sent to the dehydration tank 1 through the water or dry air introduction line 23.
- a drying step for drying the adsorbed moisture It is preferable to have a drying step for drying the adsorbed moisture.
- the gas generated by the drying process contains a small amount of organic solvent, and the gas discharged from the water or dry air discharge line 26 is directly converted into a combustion device such as a direct combustion device, a catalytic combustion device, a regenerative combustion device, or activated carbon. It can process with the gas processing apparatus generally used, such as the solvent collection
- the dew point of the dry air is preferably negative. This is because the lower the dew point and the dry air, the shorter the drying time for drying the moisture from the dehydrating material.
- the apparatus can effectively and economically dehydrate and remove moisture from the organic solvent containing moisture.
- moisture in the organic solvent can be removed stably at a low cost and with a high capacity.
- the matrix structure of the cation exchange resin is at least one selected from the group consisting of acrylic acid-based polymers, methacrylic acid-based polymers, and styrene-divinylbenzene copolymers.
- the matrix structure includes a carboxylic acid Ca group or a sulfonic acid. It is preferable that Na group is provided.
- the organic solvent that can be dehydrated in this embodiment is not particularly limited, such as ethyl acetate, methyl acetate, toluene, xylene, methyl ethyl ketone, methyl isobutyl ketone, methylene chloride, chloroform, dichloromethane, and can be applied to various organic solvents. It is.
- the organic solvent that can be dehydrated in the present embodiment is an organic solvent that is recovered using a solvent recovery processing device, which contains an organic solvent discharged from a factory in various fields, such as a dry laminating process for laminating films. Can also be applied.
- the organic solvent is adsorbed by the activated carbon fiber element 44 in which the gas 41 to be processed is introduced from the fan 42 and filled in the adsorption tower 43, and the clean gas 46 is obtained.
- the adsorption process discharged into the outside air and the introduction of steam 45 into the activated carbon fiber element 44 desorbs the organic solvent, cools and condenses with the condenser 47, separates the solvent and water with the separator 48, and collects the recovered solvent 49.
- There is a desorption process and the system is capable of continuous processing by alternately performing the adsorption process and the desorption process.
- the cleaning water discharged to the cleaning water discharge path or the dry water discharging line 26 is introduced into the cleaning water introduction path water or the dry air introducing line 23.
- a washing water circulation path 51 that branches from the dry air discharge line 26 to the water tank 11 may be provided. The opening and closing of the line of the washing water circulation path 51 is controlled by a damper 52.
- Example 1 In the organic solvent dehydrating apparatus shown in FIG. 1, a spherical cation exchange resin in which the dehydrating material is modified with a sulfonic acid Na group having a base structure of a styrene-divinylbenzene copolymer having a rack strength of 8% is used, and the particle size range is 0. The particle ratio of 0.2 mm to 0.5 mm and a particle size of 0.4 mm or less was 90%.
- the spherical cation exchange resin was measured using a particle size distribution measuring instrument (HORIBA LA-950V2) based on “Particle Size Analysis Laser Diffraction Method” defined in Japanese Industrial Standard (JIS Z 8825-1). I did it.
- a water washing step 20 L / min of tap water was introduced into the dehydration tank 1 through the water or dry air introduction line 23 to wash away the solvent adhering to the dehydrating material.
- the air volume was adjusted so that the maximum pressure loss of the dehydrating tank 1 did not exceed 90 kPa, and dry heated air of 100 ° C. and 0 ° C. DP (Dew Point (dew point)) was introduced into the dehydrating tank 1.
- Example 1 the average water concentration at the outlet in the mixed solvent dehydrated in the solvent dehydration step was reduced to 0.9% by mass, as in the above 20 cycles, and the drying step at this time The dry air volume at that time was 180 m 3 / hr.
- the mixed solvent dehydrated by the organic solvent dehydrating apparatus has an average outlet water concentration of 0.9 even if the solvent dehydration process ⁇ water washing process ⁇ drying process is repeated. It was possible to maintain the mass%, and there was no deterioration in performance, and dewatering treatment was possible stably and with high efficiency.
- Example 2 In the organic solvent dehydrating apparatus shown in FIG. 1, a plurality of spherical cation exchange resins modified with sodium sulfonate group having a base structure of styrene-divinylbenzene copolymer with a dehydrating strength of 8% are used, and the particle size range is The particle ratio of 0.1 mm to 1.0 mm and a particle size of 0.4 mm or less was 90%.
- the spherical cation exchange resin was measured using a particle size distribution measuring instrument (HORIBA LA-950V2) based on “Particle Size Analysis Laser Diffraction Method” defined in Japanese Industrial Standard (JIS Z 8825-1). I did it.
- 19 kg of this cation exchange resin is filled in the dehydration tank 1, and as a solvent dehydration step, a mixed liquid of 3% by mass of water, 80% by mass of ethyl acetate and 17% by mass of n-propyl acetate is introduced at 200 L / hr as an organic solvent to be treated. It was introduced into the dehydration tank 1 from the line 3. At this time, the adsorption temperature was 30 ° C. *
- a water washing step 20 L / min of tap water was introduced into the dehydration tank 1 through the water or dry air introduction line 23 to wash away the solvent adhering to the dehydrating material.
- the air volume was adjusted so that the maximum pressure loss of the dehydrating tank 1 did not exceed 90 kPa, and dry heated air of 100 ° C. and 0 ° C. DP (Dew Point (dew point)) was introduced into the dehydrating tank 1.
- This solvent dehydration step ⁇ water washing step ⁇ drying step required 4.5 hr.
- the average water concentration at the outlet in the mixed solvent dehydrated in the solvent dehydration step was 0.95% by mass.
- the amount of drying air at the time of the drying step was 160 m 3 / hr.
- Example 2 the mixed solvent dehydrated by the organic solvent dehydrating apparatus has an average outlet water concentration of 0.95 even if the solvent dehydration step ⁇ water washing step ⁇ drying step is repeated. It was possible to maintain the mass%, and there was no performance degradation, and the dehydration process could be stably performed with high efficiency.
- Example 3 In the organic solvent dehydrating apparatus shown in FIG. 1, a plurality of spherical cation exchange resins modified with sodium sulfonate group having a base structure of styrene-divinylbenzene copolymer with a dehydrating strength of 8% are used, and the particle size range is The particle ratio of 0.38 mm to 0.4 mm and a particle size of 0.4 mm or less was 100%.
- the spherical cation exchange resin was measured using a particle size distribution measuring instrument (HORIBA LA-950V2) based on “Particle Size Analysis Laser Diffraction Method” defined in Japanese Industrial Standard (JIS Z 8825-1). I did it.
- 19 kg of this cation exchange resin is filled in the dehydration tank 1, and as a solvent dehydration step, a mixed liquid of 2% by mass of water, 88% by mass of methylene chloride, and 10% by mass of methanol is fed at 200 L / hr from the organic solvent introduction line 3 to be treated.
- the dehydration tank 1 was introduced. At this time, the adsorption temperature was 30 ° C.
- a water washing step 20 L / min of tap water was introduced into the dehydration tank 1 through the water or dry air introduction line 23 to wash away the solvent adhering to the dehydrating material.
- the air volume was adjusted so that the maximum pressure loss of the dehydrating tank 1 did not exceed 90 kPa, and dry heated air of 100 ° C. and 0 ° C. DP (Dew Point (dew point)) was introduced into the dehydrating tank 1.
- Example 3 the mixed solvent dehydrated by the organic solvent dehydrating apparatus had an outlet average water concentration of 0.5% in the dehydrated mixed solvent even when the solvent dehydration step ⁇ water washing step ⁇ drying step was repeated. It was possible to maintain the mass%, and there was no performance degradation, and the dehydration process could be stably performed with high efficiency.
- a water washing step 20 L / min of tap water was introduced into the dehydration tank 1 through the water or dry air introduction line 23 to wash away the solvent adhering to the dehydrating material.
- the air volume was adjusted so that the maximum pressure loss of the dehydrating tank 1 did not exceed 90 kPa, and dry heated air of 100 ° C. and 0 ° C. DP (Dew Point (dew point)) was introduced into the dehydrating tank 1.
- This solvent dehydration step ⁇ water washing step ⁇ drying step required 4.5 hr.
- the average water concentration at the outlet in the mixed solvent dehydrated in the solvent dehydration step was 0.9% by mass.
- the amount of drying air during the drying process at this time was 180 m 3 / hr.
- the average water concentration at the outlet of the mixed solvent dehydrated in the solvent dehydration process increased to 1.8% by mass, and the amount of drying air at the time of the drying process was 100 m 3. / Hr.
- the mixed solvent dehydrated by the organic solvent dehydrating apparatus is an outlet in the mixed solvent dehydrated in the solvent dehydration process when the solvent dehydration process ⁇ water washing process ⁇ drying process is repeated. The average moisture concentration increases.
- the dehydrating material used is a plurality of spherical cation exchange resins modified with Na sulfonic acid group based on styrene-divinylbenzene copolymer with a dehydrating strength of 8% and a particle size range of 0.6 mm. Since the particle ratio of 0.7 mm and particle size of 0.4 mm or less was 0%, there were many cation exchange resin particles destroyed in the drying process. As a result of the clogging of the filter, it is considered that the dewatering ability of the organic solvent dewatering device was lowered.
- Comparative Example 2 In the organic solvent dehydrating apparatus shown in FIG. 1, a plurality of spherical cation exchange resins modified with Na sulfonate group having a base structure of styrene-divinylbenzene copolymer with a dehydrating strength of 8% are used. The particle ratio of 0.35 mm to 0.5 mm and a particle size of 0.4 mm or less was 80%.
- the spherical cation exchange resin was measured using a particle size distribution measuring instrument (HORIBA LA-950V2) based on “Particle Size Analysis Laser Diffraction Method” defined in Japanese Industrial Standard (JIS Z 8825-1). I did it.
- 19 kg of this cation exchange resin is filled in the dehydration tank 1, and as a solvent dehydration step, a mixed liquid of 3% by mass of water, 80% by mass of ethyl acetate and 17% by mass of n-propyl acetate is introduced at 200 L / hr as an organic solvent to be treated. It was introduced into the dehydration tank 1 from the line 3. At this time, the adsorption temperature was 30 ° C.
- a water washing step 20 L / min of tap water was introduced into the dehydration tank 1 through the water or dry air introduction line 23 to wash away the solvent adhering to the dehydrating material.
- the air volume was adjusted so that the maximum pressure loss of the dehydrating tank 1 did not exceed 90 kPa, and dry heated air of 100 ° C. and 0 ° C. DP (Dew Point (dew point)) was introduced into the dehydrating tank 1.
- the dehydrating material is made of a plurality of spherical cation exchange resins modified with Na sulfonic acid group having a base structure of styrene-divinylbenzene copolymer with a dehydrating strength of 8%.
- the particle size range is 0.35 mm. Since the particle rate of 0.5 mm and particle size of 0.4 mm or less was 80%, there were many cation exchange resin particles destroyed in the drying process. As a result of the clogging of the obtained filter, it is considered that the dewatering ability of the organic solvent dewatering device was lowered.
- 19 kg of this cation exchange resin is filled in the dehydration tank 1, and as a solvent dehydration step, a mixed liquid of 2% by mass of water, 88% by mass of methylene chloride, and 10% by mass of methanol is fed from the organic solvent introduction line 3 at 200 L / hr.
- the dehydration tank 1 was introduced. At this time, the adsorption temperature was 30 ° C.
- a water washing step 20 L / min of tap water was introduced into the dehydration tank 1 through the water or dry air introduction line 23 to wash away the solvent adhering to the dehydrating material.
- the air volume was adjusted so that the maximum pressure loss of the dehydrating tank 1 did not exceed 90 kPa, and dry heated air of 100 ° C. and 0 ° C. DP (Dew Point (dew point)) was introduced into the dehydrating tank 1.
- This solvent dehydration step ⁇ water washing step ⁇ drying step required 4.5 hr.
- the average water concentration at the outlet in the mixed solvent dehydrated in the solvent dehydration step was 0.5 mass%.
- the amount of drying air at the time of the drying process at this time was 220 m 3 / hr.
- the average water concentration at the outlet in the mixed solvent dehydrated in the solvent dehydration process increased to 0.9% by mass, and the amount of drying air at the time of the drying process was 170 m 3. / Hr.
- the mixed solvent dehydrated by the organic solvent dehydrator is the outlet in the mixed solvent dehydrated in the solvent dehydration step when the solvent dehydration step ⁇ water washing step ⁇ drying step is repeated.
- the average moisture concentration increases.
- the dehydrating material is made of a plurality of spherical cation exchange resins modified with Na sulfonic acid group having a base structure of styrene-divinylbenzene copolymer with a dehydrating strength of 8%.
- the particle size range is 0.1 mm. Since the particle ratio of 1.0 mm to 0.4 mm in particle size was 80%, there were many cation exchange resin particles destroyed in the drying process. As a result of the clogging of the obtained filter, it is considered that the dewatering ability of the organic solvent dewatering device was lowered.
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- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
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- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Drying Of Gases (AREA)
Abstract
Priority Applications (3)
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KR1020137021914A KR101762474B1 (ko) | 2011-02-21 | 2012-02-21 | 유기 용제 탈수 장치 |
CN201280009817.4A CN103402596B (zh) | 2011-02-21 | 2012-02-21 | 有机溶剂脱水装置 |
JP2012524984A JP5207014B2 (ja) | 2011-02-21 | 2012-02-21 | 有機溶剤脱水装置 |
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JP2011034626 | 2011-02-21 | ||
JP2011-034626 | 2011-02-21 |
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WO2012115081A1 true WO2012115081A1 (fr) | 2012-08-30 |
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PCT/JP2012/054058 WO2012115081A1 (fr) | 2011-02-21 | 2012-02-21 | Dispositif de déshydratation de solvant organique |
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JP (2) | JP5207014B2 (fr) |
KR (1) | KR101762474B1 (fr) |
CN (1) | CN103402596B (fr) |
WO (1) | WO2012115081A1 (fr) |
Cited By (1)
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CN112789110A (zh) * | 2019-01-30 | 2021-05-11 | 奥加诺株式会社 | 离子交换树脂的预处理装置和离子交换树脂的预处理方法 |
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CN110255659A (zh) * | 2019-07-23 | 2019-09-20 | 山东先声生物制药有限公司 | 一种浓缩处理医药废液的设备及其方法 |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS61178929A (ja) * | 1985-02-04 | 1986-08-11 | Hitachi Ltd | 塩化炭化水素系有機溶晶の全自動脱水装置 |
JPS61263608A (ja) * | 1985-05-10 | 1986-11-21 | エルフ・フランス | 炭化水素とアルコールとの混合物から成る燃料物質処理方法と水分選択吸着剤 |
JPH0440367A (ja) * | 1990-06-05 | 1992-02-10 | Mitsui Toatsu Chem Inc | 球状分離剤 |
JP2009291676A (ja) * | 2008-06-03 | 2009-12-17 | Toyobo Co Ltd | 溶剤精製装置 |
Family Cites Families (2)
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JPS61171507A (ja) * | 1985-01-24 | 1986-08-02 | Mitsubishi Chem Ind Ltd | 有機溶剤の精製法 |
JP2000225316A (ja) * | 1999-02-05 | 2000-08-15 | Ricoh Co Ltd | 溶剤ガス回収方法及び回収装置 |
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2012
- 2012-02-21 JP JP2012524984A patent/JP5207014B2/ja active Active
- 2012-02-21 WO PCT/JP2012/054058 patent/WO2012115081A1/fr active Application Filing
- 2012-02-21 CN CN201280009817.4A patent/CN103402596B/zh active Active
- 2012-02-21 KR KR1020137021914A patent/KR101762474B1/ko active IP Right Grant
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Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS61178929A (ja) * | 1985-02-04 | 1986-08-11 | Hitachi Ltd | 塩化炭化水素系有機溶晶の全自動脱水装置 |
JPS61263608A (ja) * | 1985-05-10 | 1986-11-21 | エルフ・フランス | 炭化水素とアルコールとの混合物から成る燃料物質処理方法と水分選択吸着剤 |
JPH0440367A (ja) * | 1990-06-05 | 1992-02-10 | Mitsui Toatsu Chem Inc | 球状分離剤 |
JP2009291676A (ja) * | 2008-06-03 | 2009-12-17 | Toyobo Co Ltd | 溶剤精製装置 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112789110A (zh) * | 2019-01-30 | 2021-05-11 | 奥加诺株式会社 | 离子交换树脂的预处理装置和离子交换树脂的预处理方法 |
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KR101762474B1 (ko) | 2017-07-27 |
JPWO2012115081A1 (ja) | 2014-07-07 |
CN103402596B (zh) | 2015-07-29 |
JP2013126664A (ja) | 2013-06-27 |
JP5527447B2 (ja) | 2014-06-18 |
KR20140006895A (ko) | 2014-01-16 |
JP5207014B2 (ja) | 2013-06-12 |
CN103402596A (zh) | 2013-11-20 |
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