WO2012120948A1 - Method for removing organic solvent, and removal device - Google Patents

Method for removing organic solvent, and removal device Download PDF

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Publication number
WO2012120948A1
WO2012120948A1 PCT/JP2012/052628 JP2012052628W WO2012120948A1 WO 2012120948 A1 WO2012120948 A1 WO 2012120948A1 JP 2012052628 W JP2012052628 W JP 2012052628W WO 2012120948 A1 WO2012120948 A1 WO 2012120948A1
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Prior art keywords
adsorption tank
organic solvent
gas
adsorption
acf
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PCT/JP2012/052628
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French (fr)
Japanese (ja)
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悦道 森川
武登 秦
雅英 大前
一也 篠原
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東邦化工建設株式会社
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Priority to KR1020137016707A priority Critical patent/KR101715826B1/en
Publication of WO2012120948A1 publication Critical patent/WO2012120948A1/en

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B01D53/0407—Constructional details of adsorbing systems
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/68—Halogens or halogen compounds
    • B01D53/70—Organic halogen compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26—Drying gases or vapours
    • B01D53/261—Drying gases or vapours by adsorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26—Drying gases or vapours
    • B01D53/265—Drying gases or vapours by refrigeration (condensation)
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/30—Active carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/102—Carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/30—Physical properties of adsorbents
    • B01D2253/302—Dimensions
    • B01D2253/306—Surface area, e.g. BET-specific surface
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/30—Physical properties of adsorbents
    • B01D2253/302—Dimensions
    • B01D2253/308—Pore size
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/30—Physical properties of adsorbents
    • B01D2253/302—Dimensions
    • B01D2253/311—Porosity, e.g. pore volume
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/30—Physical properties of adsorbents
    • B01D2253/34—Specific shapes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/20—Halogens or halogen compounds
    • B01D2257/206—Organic halogen compounds
    • B01D2257/2064—Chlorine
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/704—Solvents not covered by groups B01D2257/702 - B01D2257/7027
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/80—Water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/40011—Methods relating to the process cycle in pressure or temperature swing adsorption
    • B01D2259/40043—Purging
    • B01D2259/4005—Nature of purge gas
    • B01D2259/40056—Gases other than recycled product or process gas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/40083—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption
    • B01D2259/40088—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating
    • B01D2259/4009—Regeneration of adsorbents in processes other than pressure or temperature swing adsorption by heating using hot gas
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/404—Further details for adsorption processes and devices using four beds
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2

Definitions

  • the present invention relates to a method and an apparatus for removing an organic solvent in a gas to be treated containing an organic solvent, which is generated in a factory or the like.
  • This removal method and removal apparatus can be suitably used when removing a solvent from a gas to be treated having a relatively small flow rate containing a relatively high concentration low boiling point organic solvent.
  • An exhaust gas from a cleaning apparatus, a film coater apparatus, or the like in an electronic device manufacturing factory, a metal processing factory, or the like usually contains an organic solvent having a relatively low boiling point such as methylene chloride or trichlorethylene.
  • an organic solvent having a relatively low boiling point such as methylene chloride or trichlorethylene.
  • a solvent removal apparatus described below is known as an apparatus for removing an organic solvent from exhaust gas.
  • This apparatus has an adsorption process and a desorption process, and these processes are alternately switched to remove the organic solvent.
  • the organic solvent in the exhaust gas is adsorbed on the adsorbent and switched to the desorption process before the adsorbent adsorbed amount reaches saturation.
  • the adsorbent is regenerated by desorbing the organic solvent from the adsorbent using water vapor, and the desorbed organic solvent is recovered. The regenerated adsorbent is used again in the adsorption process.
  • ACF activated carbon fiber
  • ACF has a higher drying rate than conventional adsorbents. Since the conventional adsorbent has a low drying rate, it is necessary to add an adsorbent drying step after the desorption step with water vapor. On the other hand, as described above, ACF has a higher drying rate than the conventional adsorbent. Therefore, it is not necessary to provide a separate ACF drying step after the desorption step. In other words, using the gas to be processed, the adsorption of the organic solvent and the drying of the ACF can be performed simultaneously in the process of adsorbing the gas to be processed. As a result, when ACF is used as the adsorbent, it is not necessary to provide an ACF drying step substantially independently, and there is an advantage that it can be omitted.
  • the amount of ACF used increases in proportion to the amount of the organic solvent to be treated.
  • the flow rate of the gas to be processed relative to the amount of ACF used is relatively small. In this case, drying of the adsorbent performed simultaneously with the adsorption in the adsorption process becomes insufficient, and ACF containing a certain amount of moisture is used in the adsorption process. Since the ACF in this state has a reduced adsorption efficiency, there is a problem that the content of the organic solvent contained in the exhaust gas discharged from the solvent removal device becomes high.
  • Patent Document 1 a method of diluting a gas to be treated containing a high concentration organic solvent with outside air as described in Patent Document 1 is generally employed.
  • drying of the adsorbent in the adsorption process is promoted by the gas to be treated whose flow rate is increased by dilution with outside air.
  • the saturated adsorption amount of the organic solvent to the adsorbent is proportional to the concentration of the organic solvent contained in the gas to be treated, as will be described later. Therefore, the method of diluting the gas to be treated containing a high-concentration organic solvent with the outside air has a problem that the processing efficiency is lowered.
  • Patent Document 2 discloses a method of providing a drying step between the desorption step and the adsorption step.
  • each process is sequentially performed using three adsorption cans filled with the same amount of adsorbent in parallel.
  • equipment cost increases as a result of an increase in the amount of adsorbent used.
  • Japanese Patent No. 3183281 paragraph [0005] JP-A-61-35822 (first page, lower right column, line 4 to second page, upper left column, line 9)
  • the present invention provides a method and apparatus for removing a low-boiling organic solvent that uses ACF as an adsorbent, and enhances the removal efficiency of the organic solvent in the exhaust gas containing a high concentration of organic solvent and maximizes the adsorption ability of ACF. It is an object of the present invention to provide an organic solvent removal method and a removal device that can reduce running costs and device manufacturing costs.
  • the object of the present invention is to reduce the concentration of the organic solvent in the treated gas as compared with the prior art.
  • an organic solvent removal device that separates and removes the organic solvent (1) While comprising a 1st adsorption tank and a 2nd adsorption tank, these 2 tanks are arranged in series, (2) The mass ratio of the activated carbon fibers filled in the first adsorption tank and the second adsorption tank is determined within a predetermined range, (3) By attaching a condenser to a connecting pipe that connects the first adsorption tank and the second adsorption tank, the amount of organic solvent adsorbed increases, and the organic solvent discharge concentration at the outlet of the second adsorption tank It has been found that an organic solvent removing device capable of reducing the temperature can be realized. As a result, the present invention has been completed.
  • a first adsorption tank filled with activated carbon fibers The second adsorption tank filled with activated carbon fibers that are the same as or different from the activated carbon fibers, and the mass (M 2 ) of activated carbon fibers filled in the second adsorption tank is filled in the first adsorption tank.
  • An organic solvent removing apparatus having
  • the activated carbon fiber filled in the first adsorption tank has a specific surface area of 1200 m 2 / g to 2000 m 2 / g, an average pore diameter of 1 to 4 nm, and a total pore volume of 0.2 to 0.8 cm 3 / g.
  • the activated carbon fiber filled in the second adsorption tank has a specific surface area of 600 m 2 / g or more and less than 1400 m 2 / g, an average pore diameter of 0.5 to 3 nm, and a total pore volume of 0.1 to 0.6 cm.
  • [4] A method for removing an organic solvent in a gas to be treated using the organic solvent removing apparatus according to [1], By supplying the gas to be treated containing 3000 ppm or more of the organic solvent to the first adsorption tank and adsorbing the organic solvent to the activated carbon fiber filled therein, and drying the condensed water contained in the activated carbon fiber, A first adsorption tank treatment gas containing moisture and an organic solvent of 500 ppm or less is obtained, and then the first adsorption tank treatment gas is supplied to a condenser to condense and separate the moisture in the first adsorption tank treatment gas.
  • the first adsorption tank processing gas from which the moisture has been separated is supplied to the second adsorption tank, and the activated carbon fiber filled in the second adsorption tank contains the organic solvent contained in the first adsorption tank processing gas.
  • the organic solvent removal apparatus of the present invention employs ACF having a high drying rate as an adsorbent, and further includes a condenser in a connecting pipe that connects the first adsorption tank and the second adsorption tank. Water vapor discharged from the tank is discharged to the outside. Since the organic solvent removal apparatus of the present invention has the above configuration, the ACF in the second adsorption tank can be dried with a relatively small amount of gas in the adsorption step. As a result, the organic solvent concentration in the second adsorption tank processing gas can be reliably controlled to a low concentration of 100 ppm or less.
  • FIG. 1 is a graph showing the relationship between the concentration of the organic solvent contained in the gas to be treated and the saturated adsorption amount of the organic solvent with respect to the activated carbon fiber.
  • FIG. 2 is a system flow diagram showing an example of the organic solvent removing apparatus of the present invention.
  • FIG. 3 is a system flow diagram showing another example of the organic solvent removing apparatus of the present invention.
  • FIG. 1 is a graph (isothermal adsorption curve) showing the relationship between the concentration of the organic solvent (methylene chloride) contained in the gas to be treated and the saturated adsorption amount of the organic solvent adsorbed on the ACF.
  • the saturated adsorption amount of the organic solvent adsorbed on the ACF is proportional to the concentration of the organic solvent contained in the gas to be processed. That is, in the case of a gas to be treated containing a high concentration organic solvent, ACF exhibits a high saturation adsorption rate, and a high adsorption treatment efficiency can be expected. For example, consider the case where a phenolic ACF having a specific surface area of 1500 m 2 / g is used as the adsorbent. In this case, the saturated adsorption amount of ACF for a gas to be treated having a methylene chloride concentration of 5000 ppm or more, preferably 10,000 to 100,000 ppm can be expected to be 35% or more.
  • Desorption process a process of supplying steam to an adsorption tank filled with ACF to desorb and remove the organic solvent adsorbed on ACF;
  • Adsorption step By supplying the gas to be treated to the ACF from which the organic solvent has been desorbed and removed by supplying the steam, while the ACF in a wet state is dried by the water generated by the condensation of steam in the desorption step, A step of adsorbing an organic solvent in the processing gas to the ACF that is partially wet;
  • the adsorption process is complicated because the drying of the ACF and the adsorption of the organic solvent are performed simultaneously. In this adsorption process, a phenomenon different from the adsorption phenomenon in the case of using normal dry ACF occurs.
  • this point will be described in detail.
  • a dilution gas is mixed with the gas to be treated, and the concentration of the organic solvent contained in the gas to be treated is reduced to less than 5000 ppm, and actually less than 1000 ppm. Has been introduced.
  • the flow rate of the gas to be processed required for drying the ACF is obtained, and the organic solvent concentration at the outlet of the organic solvent adsorption tank is kept low.
  • the saturated adsorption amount of the adsorbent is reduced to about 18% with reference to FIG.
  • the gas to be treated is treated with a low concentration of the organic solvent, so that the amount of ACF adsorbed is reduced to about half.
  • the first adsorption tank processing gas containing the low concentration organic solvent discharged from the first adsorption tank is further processed in the second adsorption tank. Therefore, the to-be-processed gas containing the high concentration organic solvent can be introduced into the first adsorption tank.
  • the concentration of the organic solvent in the gas to be treated supplied to the first adsorption tank is preferably 5000 ppm or more, more preferably 10,000 to 100,000 ppm.
  • the first adsorption tank filled with ACF can draw out the adsorption amount of ACF twice as much as that of the conventional organic solvent treatment method.
  • the total amount of the ACF filling amount in the first adsorption tank and the ACF filling amount in the second adsorption tank is compared with the ACF filling amount in the conventional organic solvent adsorption tank using only one tank. To 52.5 to 62.5% by mass, and at least 60 to 62.5% by mass.
  • the organic solvent contained in the gas to be treated is not particularly limited.
  • the method for removing an organic solvent of the present invention can be preferably used as a method for removing an organic solvent having a low boiling point.
  • the low-boiling organic solvent referred to in the present invention is an organic solvent having a boiling point of 100 ° C. or lower, preferably 30 to 70 ° C. Examples of organic solvents having a boiling point of 30 to 70 ° C.
  • halogenated hydrocarbon organic solvents such as methylene chloride, chloroform and 1,1-dichloroethylene
  • ethers such as methylal and methyl-t-butyl ether
  • acetal organic solvents and methyl acetate.
  • ester organic solvents such as ethyl acetate
  • ketone organic solvents such as acetone and methyl ethyl ketone.
  • a condenser is interposed in the connecting pipe connecting the first adsorption tank and the second adsorption tank, whereby the amount of water in the first adsorption tank treatment gas is increased. This is advantageous for drying the ACF after the desorption treatment of the second adsorption tank.
  • the temperature drop of the first adsorption tank processing gas at the inlet and outlet of the condenser is preferably 15 to 35 ° C, more preferably 20 to 35 ° C.
  • the condenser removes 35 to 65% of the water content in the first adsorption tank processing gas.
  • the first adsorption tank treatment gas introduced into the second adsorption tank The flow rate is sufficient to dry the ACF in the second adsorption tank after the desorption process. Therefore, in the second adsorption tank, it is not necessary to provide a drying step independently after the desorption treatment as in the conventional method. In the adsorption step, the ACF in the second adsorption tank is quickly dried by the first adsorption tank treatment gas, and the solvent can be efficiently removed.
  • the method for removing an organic solvent of the present invention can be preferably used regardless of the flow rate of the gas to be treated introduced into the first adsorption tank. In particular, it can be suitably used even when the flow rate of the gas to be treated introduced into the first adsorption tank is relatively small.
  • the case where the gas to be treated is a relatively small flow rate in the present invention refers to a case where the flow rate of the gas to be treated is 1.0 Nm 3 / min or less with respect to 1 kg of the adsorbent.
  • the method for treating an organic solvent of the present invention exhibits particularly excellent effects when the flow rate of the gas to be treated is 1.0 Nm 3 / min or less, particularly 0.2 to 0.6 Nm 3 / min, per 1 kg of the adsorbent.
  • the method and apparatus for removing an organic solvent of the present invention realizes the purpose of increasing the use efficiency of ACF as an adsorbent, reducing the amount of ACF used, and eventually reducing the size of the apparatus. It is.
  • FIG. 2 is a system flow diagram showing an example of the organic solvent removing apparatus of the present invention.
  • the organic solvent removing apparatus of the present invention is broadly classified into a series of adsorption removing means composed of the following first adsorption tank (A) and second adsorption tank (B).
  • B a second adsorption tank in which the organic solvent contained in the gas treated in the first adsorption tank (first adsorption tank treatment gas) is adsorbed on the ACF and desorbed from the ACF by a batch process.
  • two adsorption removal means series capable of adsorption removal of organic compounds are provided.
  • one adsorption removal means series the first adsorption tank A and the second adsorption tank B
  • an operation for adsorbing an organic compound is performed in one adsorption removal means series.
  • the other adsorption removal means series first adsorption tank A ′, second adsorption tank B ′
  • an operation of desorbing and removing the adsorbed organic compound is performed.
  • an operation for adsorbing the organic compound is performed in the other adsorption removal means series.
  • first adsorption removal means series first adsorption tank A, second adsorption tank B
  • other adsorption removal means series first adsorption tank A ′, second adsorption tank B ′
  • the gas to be treated containing an organic solvent of 5000 ppm or more, preferably 10,000 to 100,000 ppm is transported by the blower 2 through the first adsorption tank introduction line 4 and filled with ACF 6 in the first adsorption tank A.
  • the first adsorption tank main body 8 is introduced.
  • Examples of such gas to be treated include exhaust gas generated in factories and workplaces.
  • the temperature of the gas to be treated is preferably 10 to 70 ° C, more preferably 20 to 50 ° C.
  • the first adsorption tank main body 8 has a cylindrical adsorption tank with the tower top and the cylinder bottom closed, and a cylindrical ACF 6 inserted therein.
  • a steam injection means 15 is inserted into the ACF 6 through a low wall on the lower side of the first adsorption tank main body 8.
  • steam is supplied into the hollow portion of the ACF 6 through the steam injection means 15.
  • the organic solvent adsorbed on the ACF 6 is desorbed.
  • the adsorption capacity of ACF6 is preferably 0.05 to 0.5 g, more preferably 0.1 to 0.4 g in terms of the amount of organic solvent adsorbed on 1 g of ACF.
  • the specific surface area of the ACF is preferably 1200 ⁇ 2000m 2 / g, more preferably 1400 ⁇ 2000m 2 / g, particularly preferably 1450 ⁇ 1600m 2 / g.
  • the adsorption amount of ACF having a large specific surface area is higher than the adsorption amount of ACF having a small specific surface area. Therefore, when the organic solvent concentration of the gas to be treated is 1000 ppm or more, it is preferable to use ACF6 having a specific surface area of 1200 m 2 / g or more. Furthermore, ACF6 having a specific surface area of 1200 m 2 / g or more can also collect high molecular weight organic compounds that could not be removed by conventional solvent removal apparatuses. However, since ACF6 having a specific surface area exceeding 2000 m 2 / g has a large average pore diameter, the interaction between the solvent molecules and the pores is weakened. As a result, solvent collection tends to be insufficient.
  • ACF6 preferably has an average pore diameter in the range of 1 to 4 nm, more preferably 3 to 4 nm.
  • ACF 6 is preferably one of the total pore volume of 0.2 ⁇ 0.8cm 3 / g, more preferably those of 0.3 ⁇ 0.6cm 3 / g, 0.5 ⁇ 0.6cm 3 / Particularly preferred is g.
  • an ACF having an average pore diameter, total pore volume, and specific surface area suitable for adsorption of the organic solvent is selected in consideration of the physical properties of the organic solvent to be adsorbed. It is preferable.
  • garlic ACFs such as polyacrylonitrile (PAN), pitch, cellulose, and phenol can be used.
  • PAN polyacrylonitrile
  • pitch pitch
  • cellulose cellulose
  • phenol phenol
  • the average pore diameter of the phenolic ACF increases as the specific surface area increases. Therefore, when a phenol-based ACF having a large specific surface area is employed, a polymer compound having a large molecular diameter can be adsorbed and desorbed without clogging the pores and without lowering the adsorption performance of ACF.
  • the first adsorption tank main body 8 is arranged in a plurality of one tank or more (two tanks in this example) according to the number of adsorption removal means series.
  • an organic solvent is adsorbed on the ACF 6 in the first adsorption tank main body 8.
  • the organic solvent is desorbed by introducing steam into the first adsorption tank main body 8 to regenerate the ACF 6 and at the same time, the organic solvent-containing first adsorption tank desorption gas is taken out of the first adsorption tank main body 8. Is done. Steam is injected into the first adsorption tank main body 8 through the first adsorption tank side steam introduction line 16, the steam valve 14, and the steam injection means 15. Note that the regenerated ACF 6 is in a wet state containing moisture condensed from the injected steam.
  • the organic solvent-containing first adsorption tank desorption gas passes through the first adsorption tank-side desorption gas valve 18 and the first adsorption tank-side recovery line 20 and is introduced into the condenser 22 together with the organic solvent-containing second adsorption tank desorption gas described later. .
  • the organic solvent-containing first adsorption tank desorption gas is cooled by cooling water in the condenser 22. By this condensation treatment, a recovered organic solvent is obtained as a condensed component.
  • the uncondensed component is mixed into the gas to be processed (FIG. 2).
  • the gas to be treated is sent to the first adsorption tank A through the first adsorption tank introduction line 4 by the blower 2.
  • the gas to be treated is adsorbed with the organic solvent by the ACF 6 and the first adsorption tank processing gas is taken out from the first adsorption tank A to the outside at the same time.
  • the operating conditions are selected so that the concentration of the organic solvent in the first adsorption tank treatment gas discharged from the first adsorption tank A is preferably 10 to 1000 ppm, more preferably 100 to 200 ppm.
  • the temperature of the first adsorption tank processing gas taken out is usually 30 to 70 ° C.
  • the first adsorption tank processing gas is sent to the condenser 25 through the first adsorption tank processing gas transport line 24 composed of a pipe connecting the first adsorption tank and the second adsorption tank.
  • the first adsorption tank treatment gas contains moisture generated when the steam injected in the desorption step is condensed to dry the ACF 6 in a wet state to near saturation.
  • the first adsorption tank processing gas containing moisture is sent to the second adsorption tank B after the vapor derived from steam is condensed and separated in the condenser 25.
  • the amount of water condensed and separated by the condenser 25 is preferably at least 30% by mass or more of the total amount of water contained in the first adsorption tank processing gas.
  • the organic solvent concentration in the first adsorption tank treatment gas becomes 500 ppm or less by the adsorption treatment in the adsorption step.
  • the organic solvent remaining in the first adsorption tank processing gas is removed by adsorption by the ACF 26, and the second adsorption tank processing gas having a reduced organic solvent concentration is discharged to the outside.
  • the second adsorption tank main body 28 is arranged in one tank or a plurality of tanks (two tanks in this example) according to the number of series.
  • the second adsorption tank main bodies 28, 28 are obtained by alternately switching the suction valves 30, 30 ′ and the discharge valves 32, 32 ′ and alternately switching the steam valves 34, 34 ′. 'Adsorption or desorption takes place alternately in any of the soots.
  • the configuration of the second adsorption tank B is substantially the same as the configuration of the first adsorption tank A.
  • ACF26 has an organic solvent adsorption amount of 1 to ACF of 0.05 to 0.5 g, preferably 0.1 to 0.4 g.
  • the specific surface area of ACF26 is preferably less than 600 meters 2 / g or more 1400 m 2 / g, more preferably less than 700 meters 2 / g or more 1400 m 2 / g, more preferably 1100 ⁇ 1350m 2 / g, 1200 ⁇ 1350m 2 / g is Particularly preferred.
  • the average pore diameter of ACF26 is preferably 0.5 to 3 nm, and the average pore diameter is more preferably 1 to 2.5 nm.
  • Total pore volume is preferably 0.1 ⁇ 0.6cm 3 / g, more preferably 0.2 ⁇ 0.4cm 3 / g.
  • the organic solvent adsorbed on the second adsorption tank main body 28 is desorbed by introducing steam into the second adsorption tank main body 28 in the desorption step.
  • the steam is sent to the second adsorption tank main body 28 through the second adsorption tank side steam introduction line 36, the steam valve 34, and the steam injection means 35.
  • the ACF 26 is regenerated, and simultaneously, an organic solvent-containing second adsorption tank desorption gas is generated.
  • the organic solvent-containing second adsorption tank desorption gas is introduced into the condenser 22 together with the organic solvent-containing first adsorption tank desorption gas through the second adsorption tank-side desorption gas valve 38 and the second adsorption tank-side recovery line 40. Sent.
  • the organic solvent-containing second adsorption tank desorption gas is subjected to a condensation process of cooling with cooling water.
  • a recovered organic solvent is obtained as a condensed component.
  • the uncondensed component is mixed into the gas to be treated and then sent to the first adsorption tank. ( Figure 2).
  • the concentration of the organic solvent in the second adsorption tank processing gas (cleaning gas) discharged out of the system is controlled to 100 ppm or less, preferably 60 ppm or less, more preferably 30 ppm or less.
  • the second adsorption tank processing gas may be introduced into a backup processing tank (not shown) to further reduce the organic solvent concentration.
  • the backup processing tank may be connected to the second adsorption tank processing gas transport line 42.
  • the backup treatment tank is not particularly limited, and examples thereof include a rotating drum type organic solvent treatment apparatus in which heat-resistant paper carrying an adsorbent is processed into a honeycomb shape having a large number of passages (Japanese Patent Laid-Open No. 9-308814).
  • Examples of the adsorbent supported in the backup processing tank include ACF and zeolite.
  • the present invention is not limited to this example, and one condenser 25 may be used by switching at the time of switching between the adsorption process and the desorption process as in the example of FIG. In the case of the example of FIG. 3, the equipment cost can be reduced.
  • the specific surface area, average pore diameter and total pore volume of ACF were measured under the conditions described below using a fully automatic gas adsorption amount measuring device (AUTOSORB-1 manufactured by Quantachrome Instruments).
  • the specific surface area was calculated from the obtained adsorption isotherm using the BET method.
  • the total pore volume was calculated by liquid conversion of the amount of adsorption near the relative pressure of 1.0.
  • Example 1 The organic solvent in the gas to be treated was removed using two series of removal apparatuses shown in FIG. The processing conditions are shown in Table 1 and below.
  • a gas to be treated containing 20000 ppm of methylene chloride (boiling point: 40 ° C.) as an organic solvent was subjected to an adsorption step at 3 Nm 3 / min for 8 minutes.
  • the ACF regeneration steam amount of 13 kg / h at a temperature of 120 ° C. was supplied to the ACFs 6 and 26 for 6 minutes, and the desorption process of the ACFs 6 and 26 was performed.
  • the gas to be treated was continuously removed by alternately performing the adsorption / desorption steps described above.
  • the ACF 6 used in the first adsorption tank A had a packed mass (M 1 ) of 5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.5 nm, and a total pore volume of 0.55 cm 3 / g. It was.
  • the ACF 26 used in the second adsorption tank B has a filling mass (M 2 ) of 0.5 kg, a specific surface area of 1300 m 2 / g, an average pore diameter of 0.5 nm, and a total pore volume of 0.3 cm 3 / g. Met.
  • the ACF filling mass ratio (M 2 / M 1 ) between the first adsorption tank A and the second adsorption tank B was 0.1.
  • ACFs 6 and 26 were phenolic ACFs (Toho Kako Construction Co., Ltd.) formed in a cylindrical shape.
  • the temperature drop at the inlet and the outlet of the condenser 25 interposed in the connecting pipe 24 connecting the first adsorption tank A and the second adsorption tank B was set to 20 ° C.
  • the concentration of the organic solvent in the second adsorption tank treatment gas (treated gas) was as low as 10 ppm, and the methylene chloride discharge was as low as 7 g / h.
  • the amount of steam used for ACF regeneration was as low as 25 kg / h, and the desorption treatment was efficient.
  • Example 2 As shown in Table 1, the same operation as in Example 1 was performed except that the specific surface area of ACF26 was 1500 m 2 / g, the average pore diameter was 1.5 nm, and the total pore volume was 0.55 cm 3 / g. .
  • the methylene chloride concentration in the treated gas was as low as 50 ppm, and the methylene chloride discharge was as low as 35 g / h.
  • the amount of steam for ACF regeneration was as low as 25 kg / h, and the desorption treatment was efficient.
  • Example 3 As shown in Table 1, operations were performed in the same manner as in Example 1 except that pitch-type ACF (manufactured by Toho Kako Construction Co., Ltd.) was used as ACFs 6 and 26.
  • pitch-type ACF manufactured by Toho Kako Construction Co., Ltd.
  • the ACF 6 used in the first adsorption tank A has a pitch with a packing mass (M 1 ) of 5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.3 nm, and a total pore volume of 0.5 cm 3 / g.
  • System ACF The ACF 26 used in the second adsorption tank B has a filling mass (M 2 ) of 0.5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.3 nm, and a total pore volume of 0.5 cm 3 / g.
  • the ACF filling mass ratio (M 2 / M 1 ) between the first adsorption tank A and the second adsorption tank B was 0.1.
  • the methylene chloride concentration in the treated gas was as low as 50 ppm, and the methylene chloride discharge was as low as 35 g / h.
  • the amount of steam for ACF regeneration was as small as 27 kg / h, and the desorption treatment was efficient.
  • Example 4 As shown in Table 1, the same operation as in Example 1 was performed except that PAN-based ACF (manufactured by Toho Kako Construction Co., Ltd.) was used as ACFs 6 and 26.
  • PAN-based ACF manufactured by Toho Kako Construction Co., Ltd.
  • the ACF 6 used in the first adsorption tank A had a packed mass (M 1 ) of 5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.3 nm, and a total pore volume of 0.5 cm 3 / g. It was.
  • the ACF 26 used in the second adsorption tank B has a filling mass (M 2 ) of 0.5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.3 nm, and a total pore volume of 0.5 cm 3 / g. Met.
  • the ACF filling mass ratio (M 2 / M 1 ) between the first adsorption tank A and the second adsorption tank B was 0.1.
  • the results of the adsorption / desorption treatment were such that the methylene chloride concentration in the treated gas was as low as 80 ppm and the methylene chloride discharge was as low as 56 g / h.
  • the amount of steam for ACF regeneration was as low as 29 kg / h, and the desorption treatment was efficient.
  • Example 5 As shown in Table 1, the same operation as in Example 1 was performed except that phenol-based ACF (manufactured by Toho Kako Construction Co.) was used for ACF6 and PAN-based ACF (manufactured by Toho Kako Construction Co.) was used for ACF26.
  • the ACF 6 used in the first adsorption tank A is a phenol having a filling mass (M 1 ) of 5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.5 nm, and a total pore volume of 0.55 cm 3 / g. System ACF.
  • the ACF 26 used in the second adsorption tank B has a filling mass (M 2 ) of 0.5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.3 nm, and a total pore volume of 0.5 cm 3 / g. PAN-based ACF.
  • the ACF filling mass ratio (M 2 / M 1 ) between the first tank A and the second adsorption tank B was 0.1.
  • the methylene chloride concentration in the treated gas was as low as 80 ppm, and the methylene chloride discharge was as low as 56 g / h.
  • the amount of steam for ACF regeneration was as small as 27 kg / h, and the desorption treatment was efficient.
  • Example 1 As shown in Table 2, the same operation as in Example 1 was carried out except that only one tank was used as the adsorption tank filled with ACF and the adsorption / desorption treatment was performed.
  • the ACF used in the organic solvent adsorption tank had a filling mass of 5.5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.5 nm, and a total pore volume of 0.55 cm 3 / g.
  • the methylene chloride concentration in the treated gas was as high as 200 ppm, and the methylene chloride discharge was as high as 140 g / h.
  • the amount of steam for ACF regeneration was as high as 33 kg / h, and the desorption treatment was inefficient.
  • Example 6 As shown in Table 2, the same operation as in Example 1 was performed except that the concentration of methylene chloride in the gas to be treated was changed to 50000 ppm.
  • the methylene chloride concentration in the treated gas was as low as 20 ppm, and the methylene chloride discharge was as low as 7 g / h.
  • Example 2 As shown in Table 2, the same operation as in Example 6 was carried out except that only one adsorption tank filled with ACF was subjected to the adsorption / desorption treatment.
  • the ACF used in the organic solvent adsorption tank had a packed mass of 8 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.5 nm, and a total pore volume of 0.55 cm 3 / g.
  • the methylene chloride concentration in the treated gas was as high as 500 ppm and the methylene chloride discharge was as high as 175 g / h, although a large amount of ACF was used as compared with Example 6. It became.
  • the amount of steam for ACF regeneration was as high as 33 kg / h, and the desorption treatment was inefficient.
  • Example 7 As shown in Table 2, the same operation as in Example 1 was performed except that a gas to be treated containing 20000 ppm of chloroform (boiling point 61 ° C.) was used as the organic solvent.
  • the chloroform concentration in the treated gas was as low as 50 ppm, and the chloroform discharge was as low as 28 g / h.
  • the amount of steam for ACF regeneration was as low as 25 kg / h, and the desorption treatment was efficient.
  • Example 3 As shown in Table 2, the same operation as in Example 7 was carried out except that only one adsorption tank filled with ACF was subjected to the adsorption / desorption treatment.
  • the ACF used in the organic solvent adsorption tank had a packed mass of 8 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.5 nm, and a total pore volume of 0.55 cm 3 / g.
  • the chloroform concentration in the treated gas was as high as 300 ppm and the chloroform discharge amount was as high as 170 g / h, even though a large amount of ACF was used as compared with Example 7. It became.
  • the amount of steam for ACF regeneration was as high as 33 kg / h, and the desorption treatment was inefficient.
  • Example 8 As shown in Table 3, the gas flow rate to be treated was 220 Nm 3 / h. The same operation as in Example 1 was performed except that the ACF filling amount was set to 6 kg for the first adsorption tank A (M 1 ) and 0.6 kg for the second adsorption tank B (M 2 ) as the gas flow increased. did. The ACF filling mass ratio (M 2 / M 1 ) between the first tank A and the second tank B was 0.1, and the whole (M 1 + M 2 ) was 6.6 kg.
  • the methylene chloride concentration in the treated gas was as low as 10 ppm, and the methylene chloride discharge was as low as 10 g / h.
  • Example 4 The amount of steam for ACF regeneration was 29 kg / h. Compared to Example 1, the amount of steam for ACF regeneration increased as the amount of ACF used increased, but the desorption efficiency was sufficiently good.
  • Example 4 As shown in Table 3, the same operation as in Example 8 was performed except that only one adsorption tank filled with ACF was subjected to the adsorption / desorption treatment.
  • the ACF used in the organic solvent adsorption tank had a filling mass of 12 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.5 nm, and a total pore volume of 0.55 cm 3 / g.
  • the amount of steam for ACF regeneration was as high as 52 kg / h, and the desorption treatment was inefficient.
  • Example 9 As shown in Table 4, the same operation as in Example 1 was performed except that the ACF filling amount was 5 kg for the first adsorption tank A (M 1 ) and 0.3 kg for the second adsorption tank B (M 2 ).
  • the ACF filling mass ratio (M 2 / M 1 ) between the first adsorption tank A and the second adsorption tank B was 0.06, and the whole (M 1 + M 2 ) was 5.3 kg.
  • the methylene chloride concentration in the treated gas was as low as 10 ppm, and the methylene chloride discharge was as low as 7 g / h.
  • the amount of steam for ACF regeneration was 23 kg / h, and the desorption treatment was efficient.
  • Example 5 As shown in Table 4, the same operation as in Example 1 was performed except that the ACF filling amount was 5 kg for the first adsorption tank A (M 1 ) and 0.2 kg for the second adsorption tank B (M 2 ).
  • the ACF filling mass ratio (M 2 / M 1 ) between the first adsorption tank A and the second adsorption tank B was 0.04, and the whole (M 1 + M 2 ) was 5.2 kg.
  • the methylene chloride concentration in the treated gas was as high as 150 ppm.
  • the methylene chloride discharge was high at 105 g / h.
  • Example 10 As shown in Table 4, the same operation as in Example 1 was performed except that the ACF filling amount was 5 kg for the first adsorption tank A (M 1 ) and 1 kg for the second adsorption tank B (M 2 ).
  • the ACF filling mass ratio (M 2 / M 1 ) between the first adsorption tank A and the second adsorption tank B was 0.2, and the whole (M 1 + M 2 ) was 6 kg.
  • the methylene chloride concentration in the treated gas was as low as 20 ppm, and the methylene chloride discharge was as low as 14 g / h.
  • the amount of steam for ACF regeneration was as low as 24 kg / h, and the desorption treatment was efficient.
  • Example 6 As shown in Table 4, the same operation as in Example 1 was performed except that the ACF filling amount was 4.5 kg for the first adsorption tank A (M 1 ) and 1.5 kg for the second adsorption tank B (M 2 ). did.
  • the amount of steam for ACF regeneration was as small as 23 kg / h, and the desorption treatment was efficient.
  • the drying of the second adsorption tank B became insufficient, and as a result, the methylene chloride concentration in the treated gas was as high as 150 ppm.
  • the methylene chloride discharge was as high as 105 g / h.
  • Example 11 As shown in Table 2 and the following conditions, the same operation as in Example 1 was performed except that a gas to be treated containing 20000 ppm methylal (boiling point 42.5 ° C.) as an organic solvent was used.
  • the methylal concentration in the treated gas was as low as 80 ppm, and the methylal discharge was as low as 49 g / h.
  • the amount of steam for ACF regeneration was 29 kg / h, and the desorption treatment was efficient.
  • Example 12 As shown in Table 2 and the following conditions, the same operation as in Example 1 was performed except that a gas to be treated containing 20000 ppm of methyl acetate (boiling point 54 ° C.) was used as the organic solvent.
  • the methyl acetate concentration in the treated gas was as low as 80 ppm and the methyl acetate discharge was as low as 48 g / h.
  • the amount of steam for ACF regeneration was as small as 28 kg / h, and the desorption treatment was efficient.
  • Example 13 As shown in Table 5, the same operation as in Example 1 was performed except that a gas to be treated containing 20000 ppm of acetone (boiling point: 56.5 ° C.) was used as the organic solvent.
  • the concentration of acetone in the treated gas was as low as 50 ppm, and the amount of acetone discharged was as low as 24 g / h.
  • the amount of steam for ACF regeneration was as small as 28 kg / h, and the desorption treatment was efficient.

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Abstract

The present invention discloses a device for removing an organic solvent, the device comprising a first adsorption tank, into which active carbon fibers are to be packed, a second adsorption tank, into which active carbon fibers that are the same as or different from said active carbon fibers are to be packed, the mass (M2) of the active carbon fibers to be packed into the second adsorption tank being 0.05-0.25 in terms of mass ratio (M2/M1) to the mass (M1) of the active carbon fibers to be packed into the first adsorption tank, a connection pipe which connects the first adsorption tank and the second adsorption tank, a condenser disposed in the connection pipe, and steam injection means respectively disposed for the first adsorption tank and the second adsorption tank.

Description

有機溶剤の除去方法、及び除去装置Method and apparatus for removing organic solvent
本発明は、工場等において発生する、有機溶剤を含む被処理ガス中の有機溶剤の除去方法及び除去装置に関する。本除去方法、及び除去装置は、比較的高濃度の低沸点有機溶剤を含む比較的小流量の被処理ガスから溶剤を除去する場合に好適に使用できる。 The present invention relates to a method and an apparatus for removing an organic solvent in a gas to be treated containing an organic solvent, which is generated in a factory or the like. This removal method and removal apparatus can be suitably used when removing a solvent from a gas to be treated having a relatively small flow rate containing a relatively high concentration low boiling point organic solvent.
電子機器製造工場、金属加工工場等における洗浄装置、フィルムコーター装置等の排ガスの中には、塩化メチレン、トリクロロエチレン等の比較的沸点の低い有機溶剤が通常含まれている。これらの有機溶剤を含有する排ガスを、そのまま大気中に放出すると、環境汚染を引き起こすので、通常大気中に放出する前に溶剤の除去処理が行われる。 An exhaust gas from a cleaning apparatus, a film coater apparatus, or the like in an electronic device manufacturing factory, a metal processing factory, or the like usually contains an organic solvent having a relatively low boiling point such as methylene chloride or trichlorethylene. When exhaust gases containing these organic solvents are released into the atmosphere as they are, environmental pollution is caused. Therefore, the solvent is usually removed before being released into the atmosphere.
　従来、排ガスから有機溶剤を除去する装置として、以下に記載する溶剤除去装置が知られている。この装置は、吸着工程と、脱着工程とを有し、これら工程を交互に切替えて有機溶剤を除去する。 Conventionally, a solvent removal apparatus described below is known as an apparatus for removing an organic solvent from exhaust gas. This apparatus has an adsorption process and a desorption process, and these processes are alternately switched to remove the organic solvent.
　吸着工程においては、排ガス中の有機溶剤を吸着材に吸着させ、吸着材の吸着量が飽和に達する前に脱着工程に切替える。脱着工程においては、水蒸気を用いて吸着材から有機溶剤を脱着させることにより吸着材を再生すると共に、脱着させた有機溶剤を回収する。再生した吸着材は、再度吸着工程において使用する。 In the adsorption process, the organic solvent in the exhaust gas is adsorbed on the adsorbent and switched to the desorption process before the adsorbent adsorbed amount reaches saturation. In the desorption step, the adsorbent is regenerated by desorbing the organic solvent from the adsorbent using water vapor, and the desorbed organic solvent is recovered. The regenerated adsorbent is used again in the adsorption process.
　有機溶剤の吸着に用いる吸着材としては、活性炭素繊維(ＡＣＦ)がある。ＡＣＦは、活性炭等の従来の吸着材に比べて溶剤の吸脱着速度の大きいので、好ましい吸着材である。 As an adsorbent used for adsorption of an organic solvent, there is activated carbon fiber (ACF). ACF is a preferred adsorbent because it has a higher solvent adsorption / desorption rate than conventional adsorbents such as activated carbon.
　更に、従来の吸着材と比べて、ＡＣＦは、乾燥速度が大きい。従来の吸着材は、乾燥速度が小さいので、水蒸気による脱着工程の後に、吸着材の乾燥工程を付加する必要がある。一方、前述のように従来の吸着材と比べて、ＡＣＦは、乾燥速度が大きい。従って、脱着工程の後のＡＣＦの乾燥工程を独立して設ける必要が無い。即ち、被処理ガスを利用して、被処理ガスの吸着工程において、有機溶剤の吸着とＡＣＦの乾燥とを同時に行うことができる。その結果、吸着材としてＡＣＦを用いる場合には、実質的にＡＣＦの乾燥工程を独立して設ける必要が無く、省略できる利点がある。 Furthermore, ACF has a higher drying rate than conventional adsorbents. Since the conventional adsorbent has a low drying rate, it is necessary to add an adsorbent drying step after the desorption step with water vapor. On the other hand, as described above, ACF has a higher drying rate than the conventional adsorbent. Therefore, it is not necessary to provide a separate ACF drying step after the desorption step. In other words, using the gas to be processed, the adsorption of the organic solvent and the drying of the ACF can be performed simultaneously in the process of adsorbing the gas to be processed. As a result, when ACF is used as the adsorbent, it is not necessary to provide an ACF drying step substantially independently, and there is an advantage that it can be omitted.
　しかし、高濃度の有機溶剤を含む小流量の被処理ガスから有機溶剤を除去する場合、処理すべき有機溶剤の量に比例してＡＣＦの使用量は増加する。更に、高濃度の有機溶剤を含む小流量の被処理ガスを処理する場合、ＡＣＦの使用量に対する被処理ガスの流量が相対的に少なくなる。この場合は、吸着工程で吸着と同時に行われる吸着材の乾燥が不充分になり、ある程度水分を含む状態のＡＣＦが吸着工程において使用されることになる。この状態のＡＣＦは、吸着効率が低下しているので、溶剤除去装置から排出される排出ガスに含まれる有機溶剤の含有量が高くなる問題がある。 However, when the organic solvent is removed from the gas having a small flow rate containing a high concentration organic solvent, the amount of ACF used increases in proportion to the amount of the organic solvent to be treated. Further, when processing a small amount of gas to be processed containing a high-concentration organic solvent, the flow rate of the gas to be processed relative to the amount of ACF used is relatively small. In this case, drying of the adsorbent performed simultaneously with the adsorption in the adsorption process becomes insufficient, and ACF containing a certain amount of moisture is used in the adsorption process. Since the ACF in this state has a reduced adsorption efficiency, there is a problem that the content of the organic solvent contained in the exhaust gas discharged from the solvent removal device becomes high.
　この問題を改善するために、特許文献１に記載されるような、高濃度有機溶剤を含む被処理ガスを外気で希釈する方法が一般的に採用されている。この方法は、外気で希釈することによって流量を増大させた被処理ガスによって、吸着工程にある吸着材の乾燥を促進させる方法である。 In order to improve this problem, a method of diluting a gas to be treated containing a high concentration organic solvent with outside air as described in Patent Document 1 is generally employed. In this method, drying of the adsorbent in the adsorption process is promoted by the gas to be treated whose flow rate is increased by dilution with outside air.
　しかし、吸着材に対する有機溶剤の飽和吸着量は、後述のように、被処理ガスに含まれる有機溶剤の濃度に比例する。従って、高濃度の有機溶剤を含む被処理ガスを外気により希釈する方法は、処理効率の低下の問題がある。 However, the saturated adsorption amount of the organic solvent to the adsorbent is proportional to the concentration of the organic solvent contained in the gas to be treated, as will be described later. Therefore, the method of diluting the gas to be treated containing a high-concentration organic solvent with the outside air has a problem that the processing efficiency is lowered.
　特許文献２には、脱着工程と吸着工程の間に乾燥工程を設ける方法が開示されている。しかし、この方法においては、同量の吸着材を充填した吸着缶を並列に３つ使用して順次各工程を行うことになる。この場合は、使用する吸着材の量が増加する結果、設備コストが増加する問題がある。
特許第３１８３３８１号公報  (段落［０００５］) 特開昭６１－３５８２２号公報  (第１頁右下欄第４行～第２頁左上欄第９行) Patent Document 2 discloses a method of providing a drying step between the desorption step and the adsorption step. However, in this method, each process is sequentially performed using three adsorption cans filled with the same amount of adsorbent in parallel. In this case, there is a problem that equipment cost increases as a result of an increase in the amount of adsorbent used.
Japanese Patent No. 3183281 (paragraph [0005]) JP-A-61-35822 (first page, lower right column, line 4 to second page, upper left column, line 9)
　本発明は、吸着材としてＡＣＦ用いる低沸点有機溶剤の除去方法、及び除去装置において、高濃度の有機溶剤を含有する排ガス中の有機溶剤の除去効率を高めると共に、ＡＣＦの持つ吸着能力を最大化させることにより、ランニングコスト及び装置製作費用を縮減させる有機溶剤の除去方法、及び除去装置を提供することを目的としている。 The present invention provides a method and apparatus for removing a low-boiling organic solvent that uses ACF as an adsorbent, and enhances the removal efficiency of the organic solvent in the exhaust gas containing a high concentration of organic solvent and maximizes the adsorption ability of ACF. It is an object of the present invention to provide an organic solvent removal method and a removal device that can reduce running costs and device manufacturing costs.
　即ち、処理済ガス中の有機溶剤濃度が従来技術と同等の場合は、吸着槽に充填されるＡＣＦの全体量を縮減できること、吸着槽に充填されるＡＣＦの全体量が従来技術と同等の場合は、処理済ガス中の有機溶剤濃度を従来技術よりも低減できることを、本発明は目的としている。 That is, when the concentration of the organic solvent in the treated gas is equivalent to that of the prior art, the total amount of ACF filled in the adsorption tank can be reduced, and the total amount of ACF filled in the adsorption tank is equivalent to that of the conventional technique. The object of the present invention is to reduce the concentration of the organic solvent in the treated gas as compared with the prior art.
　本発明者は、上記課題を解決するために、活性炭素繊維を用いる有機溶剤除去装置について検討を重ねた。その結果、有機溶剤を分離除去する有機溶剤除去装置を、
（１）第１吸着槽と第２吸着槽とで構成すると共に、これら２槽を直列に配置し、
（２）第１吸着槽と第２吸着槽とに充填される活性炭素繊維の質量比を所定の範囲に定め、
（３）前記第１吸着槽と第２吸着槽とを連結する連結管に凝縮器を介装する、ことにより、有機溶剤の吸着量が増加し、且つ第２吸着槽出口の有機溶剤排出濃度を低下することのできる有機溶剤の除去装置を実現できることを見出した。その結果、本発明を完成するに到った。 In order to solve the above-mentioned problems, the present inventor has repeatedly studied an organic solvent removing apparatus using activated carbon fibers. As a result, an organic solvent removal device that separates and removes the organic solvent
(1) While comprising a 1st adsorption tank and a 2nd adsorption tank, these 2 tanks are arranged in series,
(2) The mass ratio of the activated carbon fibers filled in the first adsorption tank and the second adsorption tank is determined within a predetermined range,
(3) By attaching a condenser to a connecting pipe that connects the first adsorption tank and the second adsorption tank, the amount of organic solvent adsorbed increases, and the organic solvent discharge concentration at the outlet of the second adsorption tank It has been found that an organic solvent removing device capable of reducing the temperature can be realized. As a result, the present invention has been completed.
　上記課題を解決する本発明は以下に記載するものである。 The present invention for solving the above-mentioned problems is described below.
  〔１〕　活性炭素繊維が充填される第１吸着槽と、
　前記活性炭素繊維と同一又は異なる活性炭素繊維が充填される第２吸着槽であって、第２吸着槽に充填される活性炭素繊維の質量(Ｍ２)が、第１吸着槽に充填される活性炭素繊維の質量(Ｍ１)を基準として、質量比(Ｍ２／Ｍ１)で０．０５～０．２５である第２吸着槽と、
　前記第１吸着槽と、第２吸着槽とを連結する連結管と、
　前記連結管に介装される凝縮器と、
　前記第１吸着槽及び第２吸着槽にそれぞれ設けられるスチーム注入手段と、
　を有する有機溶剤の除去装置。 [1] a first adsorption tank filled with activated carbon fibers;
The second adsorption tank filled with activated carbon fibers that are the same as or different from the activated carbon fibers, and the mass (M 2 ) of activated carbon fibers filled in the second adsorption tank is filled in the first adsorption tank. A second adsorption tank having a mass ratio (M 2 / M 1 ) of 0.05 to 0.25 on the basis of the mass (M 1 ) of the activated carbon fiber;
A connecting pipe connecting the first adsorption tank and the second adsorption tank;
A condenser interposed in the connecting pipe;
Steam injection means provided in each of the first adsorption tank and the second adsorption tank;
An organic solvent removing apparatus having
　〔２〕　第１吸着槽に充填される活性炭素繊維が、比表面積１２００ｍ２／ｇ～２０００ｍ２／ｇ、平均細孔直径１～４ｎｍ、全細孔容積０．２～０．８ｃｍ３／ｇの活性炭素繊維である〔１〕に記載の有機溶剤の除去装置。 [2] The activated carbon fiber filled in the first adsorption tank has a specific surface area of 1200 m 2 / g to 2000 m 2 / g, an average pore diameter of 1 to 4 nm, and a total pore volume of 0.2 to 0.8 cm 3 / g. The organic solvent removing apparatus according to [1], which is an activated carbon fiber.
　〔３〕　第２吸着槽に充填される活性炭素繊維が、比表面積６００ｍ２／ｇ以上１４００ｍ２／ｇ未満、平均細孔直径０．５～３ｎｍ、全細孔容積０．１～０．６ｃｍ３／ｇの活性炭素繊維である〔１〕に記載の有機溶剤の除去装置。 [3] The activated carbon fiber filled in the second adsorption tank has a specific surface area of 600 m 2 / g or more and less than 1400 m 2 / g, an average pore diameter of 0.5 to 3 nm, and a total pore volume of 0.1 to 0.6 cm. The organic solvent removing apparatus according to [1], which is 3 / g of activated carbon fiber.
　〔４〕　〔１〕に記載の有機溶剤の除去装置を用いる被処理ガス中の有機溶剤の除去方法であって、
　有機溶剤を３０００ｐｐｍ以上含む被処理ガスを第１吸着槽に供給してその内部に充填される活性炭素繊維に有機溶剤を吸着させると共に、活性炭素繊維に含まれる凝縮水の乾燥を行うことにより、水分と５００ｐｐｍ以下の有機溶剤とを含む第１吸着槽処理ガスを得、次いでこの第１吸着槽処理ガスを凝縮器に供給して第１吸着槽処理ガス中の水分を凝縮分離して系外に排出すると共に、前記水分を分離した第１吸着槽処理ガスを第２吸着槽に供給して、第２吸着槽の内部に充填される活性炭素繊維に第１吸着槽処理ガスが含む有機溶剤を吸着させると共に、この活性炭素繊維が含む水分を乾燥させることにより、有機溶剤濃度が１００ｐｐｍ以下の第２吸着槽処理ガスを系外に排出させる吸着工程と、
　第１吸着槽に供給する被処理ガスの供給を停止した後、スチーム注入手段により第１吸着槽及び第２吸着槽内にスチームを供給して、第１吸着槽及び第２吸着槽内に充填されている各活性炭素繊維が吸着している有機溶剤を脱着させることにより、前記有機溶剤を吸着している各活性炭素繊維を、前記供給したスチームが凝縮して生じる凝縮水を含む活性炭素繊維に、再生させると共に、前記脱着させた有機溶剤を系外に取出す脱着工程と、
　を交互に繰返す被処理ガス中の有機溶剤の除去方法。 [4] A method for removing an organic solvent in a gas to be treated using the organic solvent removing apparatus according to [1],
By supplying the gas to be treated containing 3000 ppm or more of the organic solvent to the first adsorption tank and adsorbing the organic solvent to the activated carbon fiber filled therein, and drying the condensed water contained in the activated carbon fiber, A first adsorption tank treatment gas containing moisture and an organic solvent of 500 ppm or less is obtained, and then the first adsorption tank treatment gas is supplied to a condenser to condense and separate the moisture in the first adsorption tank treatment gas. And the first adsorption tank processing gas from which the moisture has been separated is supplied to the second adsorption tank, and the activated carbon fiber filled in the second adsorption tank contains the organic solvent contained in the first adsorption tank processing gas. An adsorption step of discharging the second adsorption tank processing gas having an organic solvent concentration of 100 ppm or less to the outside by drying the moisture contained in the activated carbon fiber.
After the supply of the gas to be processed to be supplied to the first adsorption tank is stopped, steam is supplied into the first adsorption tank and the second adsorption tank by the steam injection means, and the first adsorption tank and the second adsorption tank are filled. Activated carbon fibers containing condensed water produced by the condensation of the supplied steam by desorbing the organic solvent adsorbed by each activated carbon fiber being adsorbed to each activated carbon fiber adsorbing the organic solvent And a desorption step of regenerating and taking out the desorbed organic solvent out of the system,
The method of removing the organic solvent in the gas to be processed that repeats alternately.
　〔５〕　凝縮器の入口と出口とにおける第１吸着槽処理ガスの温度降下を１５～３５℃に保つことにより、第１吸着槽処理ガス中の水分量の３５～６５％を除去する〔４〕に記載の有機溶剤の除去方法。 [5] 35 to 65% of the moisture content in the first adsorption tank treatment gas is removed by maintaining the temperature drop of the first adsorption tank treatment gas at the inlet and outlet of the condenser at 15 to 35 ° C. [4 ] The removal method of the organic solvent of description.
　〔６〕　第１吸着槽に供給する被処理ガスが、沸点が３０～７０℃の有機溶剤を５０００～１０００００ｐｐｍ含む被処理ガスである〔４〕に記載の有機溶剤の除去方法。 [6] The method for removing an organic solvent according to [4], wherein the gas to be treated supplied to the first adsorption tank is a gas to be treated containing 5000 to 100,000 ppm of an organic solvent having a boiling point of 30 to 70 ° C.
　本発明の有機溶剤の除去装置は、吸着材として乾燥速度の大きいＡＣＦを採用し、更には前記第１吸着槽と第２吸着槽とを連結する連結管に凝縮器を備えて、第１吸着槽が排出する水蒸気を外部に排出している。本発明の有機溶剤の除去装置は、上記構成を有するので、吸着工程において比較的少量のガスで、第２吸着槽のＡＣＦを乾燥できる。その結果、第２吸着槽処理ガス中の有機溶剤濃度を確実に１００ｐｐｍ以下の低濃度に制御できる。 The organic solvent removal apparatus of the present invention employs ACF having a high drying rate as an adsorbent, and further includes a condenser in a connecting pipe that connects the first adsorption tank and the second adsorption tank. Water vapor discharged from the tank is discharged to the outside. Since the organic solvent removal apparatus of the present invention has the above configuration, the ACF in the second adsorption tank can be dried with a relatively small amount of gas in the adsorption step. As a result, the organic solvent concentration in the second adsorption tank processing gas can be reliably controlled to a low concentration of 100 ppm or less.
図１は、被処理ガスに含まれる有機溶剤濃度と、活性炭素繊維に対する有機溶剤の飽和吸着量との関係を示すグラフである。FIG. 1 is a graph showing the relationship between the concentration of the organic solvent contained in the gas to be treated and the saturated adsorption amount of the organic solvent with respect to the activated carbon fiber. 図２は、本発明の有機溶剤の除去装置の一例を示すシステムフロー図である。FIG. 2 is a system flow diagram showing an example of the organic solvent removing apparatus of the present invention. 図３は、本発明の有機溶剤の除去装置の他の例を示すシステムフロー図である。FIG. 3 is a system flow diagram showing another example of the organic solvent removing apparatus of the present invention.
Ａ、Ａ’    第１吸着槽
  Ｂ、Ｂ’    第２吸着槽
  ２    ブロワ
  ４    第１吸着槽導入ライン
  ６、６’、２６、２６’    ＡＣＦ
  ８、８’    第１吸着槽主体
  １０、１０’、３０、３０’    吸入バルブ
  １２、１２’、３２、３２’    排出バルブ
  １４、１４’、３４、３４’    蒸気バルブ
  １５、１５’、３５、３５’    スチーム注入手段
  １６    第１吸着槽側スチーム導入ライン
  １８    第１吸着槽側脱着ガスバルブ
  ２０    第１吸着槽側回収ライン
  ２２、２５、２５’    凝縮器
  ２４    第１吸着槽処理ガス輸送ライン
  ２８、２８’    第２吸着槽主体
  ３６    第２吸着槽側スチーム導入ライン
  ３８    第２吸着槽側脱着ガスバルブ
  ４０    第２吸着槽側回収ライン
  ４２    第２吸着槽処理ガス輸送ライン A, A ′ first adsorption tank B, B ′ second adsorption tank 2 blower 4 first adsorption tank introduction line 6, 6 ′, 26, 26 ′ ACF
8, 8 'First adsorption tank main body 10, 10', 30, 30 ' Suction valve 12, 12', 32, 32 ' Discharge valve 14, 14', 34, 34 ' Steam valve 15, 15', 35, 35 'Steam injection means 16 First adsorption tank side steam introduction line 18 First adsorption tank side desorption gas valve 20 First adsorption tank side recovery line 22, 25, 25' Condenser 24 First adsorption tank processing gas transport line 28, 28 ' Second adsorption tank main body 36 Second adsorption tank side steam introduction line 38 Second adsorption tank side desorption gas valve 40 Second adsorption tank side recovery line 42 Second adsorption tank processing gas transport line
以下、図面を参照しながら、本発明を詳細に説明する。 Hereinafter, the present invention will be described in detail with reference to the drawings.
  図１は、被処理ガスに含まれる有機溶剤(塩化メチレン)濃度と、ＡＣＦに吸着する有機溶剤の飽和吸着量との関係を示すグラフ（等温吸着曲線）である。 FIG. 1 is a graph (isothermal adsorption curve) showing the relationship between the concentration of the organic solvent (methylene chloride) contained in the gas to be treated and the saturated adsorption amount of the organic solvent adsorbed on the ACF.
　図１に示すように、ＡＣＦに吸着する有機溶剤の飽和吸着量は、被処理ガスに含まれる有機溶剤濃度に比例する。即ち、高濃度の有機溶剤を含有する被処理ガスの場合に、ＡＣＦは高い飽和吸着率を示し、高い吸着処理効率が期待できる。例えば、吸着材として比表面積１５００ｍ２／ｇのフェノール系ＡＣＦを使用する場合を考える。この場合、塩化メチレン濃度が５０００ｐｐｍ以上、好ましくは１００００～１０００００ｐｐｍの被処理ガスに対するＡＣＦの飽和吸着量は３５％以上が見込める。 As shown in FIG. 1, the saturated adsorption amount of the organic solvent adsorbed on the ACF is proportional to the concentration of the organic solvent contained in the gas to be processed. That is, in the case of a gas to be treated containing a high concentration organic solvent, ACF exhibits a high saturation adsorption rate, and a high adsorption treatment efficiency can be expected. For example, consider the case where a phenolic ACF having a specific surface area of 1500 m 2 / g is used as the adsorbent. In this case, the saturated adsorption amount of ACF for a gas to be treated having a methylene chloride concentration of 5000 ppm or more, preferably 10,000 to 100,000 ppm can be expected to be 35% or more.
　以下、下記、吸着工程と、脱着工程とを交互に繰返す、有機溶剤の除去方法について考える。
脱着工程：　ＡＣＦが充填されている吸着槽にスチームを供給して、ＡＣＦに吸着されている有機溶剤を脱着除去する工程、
吸着工程：　前記スチームを供給して有機溶剤を脱着除去したＡＣＦに被処理ガスを供給することにより、前記脱着工程においてスチームが凝縮して生成する水により湿潤状態にあるＡＣＦを乾燥させながら、被処理ガス中の有機溶剤を、一部湿潤状態にあるＡＣＦに吸着させる工程、
上記の、一部湿潤状態にあるＡＣＦを用いる有機溶剤の除去方法にあっては、吸着工程は、ＡＣＦの乾燥と、有機溶剤の吸着が同時に行われるので、吸着現象は複雑である。この吸着工程は、通常の乾燥したＡＣＦを用いる場合の吸着現象とは異なる現象が起きる。　以下、この点について詳述する。 Hereinafter, a method for removing an organic solvent in which an adsorption process and a desorption process described below are alternately repeated will be considered.
Desorption process: a process of supplying steam to an adsorption tank filled with ACF to desorb and remove the organic solvent adsorbed on ACF;
Adsorption step: By supplying the gas to be treated to the ACF from which the organic solvent has been desorbed and removed by supplying the steam, while the ACF in a wet state is dried by the water generated by the condensation of steam in the desorption step, A step of adsorbing an organic solvent in the processing gas to the ACF that is partially wet;
In the method for removing an organic solvent using ACF that is partially wet as described above, the adsorption process is complicated because the drying of the ACF and the adsorption of the organic solvent are performed simultaneously. In this adsorption process, a phenomenon different from the adsorption phenomenon in the case of using normal dry ACF occurs. Hereinafter, this point will be described in detail.
　ＡＣＦを用いて被処理ガスから有機溶剤を吸着除去する場合、一般に、被処理ガス中の有機溶剤の濃度が高くなると、吸着すべき有機溶剤の量が増加するので、ＡＣＦの使用量は増加する。この場合は、ＡＣＦの使用量に対する被処理ガスの流量は相対的に少なくなる。その結果、吸着工程において、湿潤状態のＡＣＦを乾燥させるのに必要な被処理ガス流量が不足し、ＡＣＦの水分乾燥が不十分になる。この場合は、特に吸着工程の初期における有機溶剤の吸着効率が低下してしまう。 When an organic solvent is adsorbed and removed from a gas to be treated using ACF, generally, when the concentration of the organic solvent in the gas to be treated increases, the amount of the organic solvent to be adsorbed increases, so the amount of ACF used increases. . In this case, the flow rate of the gas to be processed relative to the amount of ACF used is relatively small. As a result, in the adsorption step, the flow rate of the gas to be processed necessary for drying the wet ACF is insufficient, and the moisture drying of the ACF is insufficient. In this case, the adsorption efficiency of the organic solvent particularly in the initial stage of the adsorption step is lowered.
　即ち、上記吸着工程と脱着工程を交互に行う有機溶剤の除去方法に使用するＡＣＦの有機溶剤飽和吸着量とＡＣＦの含水量との間には、ある平衡関係が存在する。その結果、ＡＣＦの含水量と、吸着槽の出口から排出される処理ガス中の有機溶剤濃度は、平衡値に保たれる。 That is, there is a certain equilibrium relationship between the saturated adsorption amount of organic solvent of ACF and the water content of ACF used in the organic solvent removal method in which the adsorption step and the desorption step are alternately performed. As a result, the water content of ACF and the concentration of the organic solvent in the processing gas discharged from the outlet of the adsorption tank are maintained at an equilibrium value.
　従来の有機溶剤処理方法においては、被処理ガスに希釈ガスを混合し、被処理ガスに含まれる有機溶剤濃度を５０００ｐｐｍ未満、実際には１０００ｐｐｍ以下の低濃度にした後、これを有機溶剤吸着槽に導入している。この操作により、ＡＣＦを乾燥させるのに必要な被処理ガスの流量を得ると共に、有機溶剤吸着槽の出口における有機溶剤濃度を低く保っている。この場合、吸着材の飽和吸着量は、図１を参照すれば１８％程度に低下している。即ち、上記従来法においては、有機溶剤濃度を低くして被処理ガスを処理しているので、ＡＣＦの吸着量をわざわざ半分程度に低下させて使用していることになる。 In the conventional organic solvent treatment method, a dilution gas is mixed with the gas to be treated, and the concentration of the organic solvent contained in the gas to be treated is reduced to less than 5000 ppm, and actually less than 1000 ppm. Has been introduced. By this operation, the flow rate of the gas to be processed required for drying the ACF is obtained, and the organic solvent concentration at the outlet of the organic solvent adsorption tank is kept low. In this case, the saturated adsorption amount of the adsorbent is reduced to about 18% with reference to FIG. In other words, in the above conventional method, the gas to be treated is treated with a low concentration of the organic solvent, so that the amount of ACF adsorbed is reduced to about half.
　一方、本発明の有機溶剤の除去方法においては、第１吸着槽から排出される低濃度の有機溶剤を含有する第１吸着槽処理ガスが、第２吸着槽で更に処理される。そのため、第１吸着槽に高濃度の有機溶剤を含む被処理ガスを導入できる。第１吸着槽に供給する被処理ガス中の有機溶剤濃度は５０００ｐｐｍ以上であることが好ましく、更に好ましくは１００００～１０００００ｐｐｍである。被処理ガス中の有機溶剤の濃度を５０００ｐｐｍ以上とすることで、図１のグラフに従って、ＡＣＦへの有機溶剤の飽和吸着量が３０％以上になる。即ち、高い吸着量を維持した状態で除去処理を行うことができる。 On the other hand, in the organic solvent removal method of the present invention, the first adsorption tank processing gas containing the low concentration organic solvent discharged from the first adsorption tank is further processed in the second adsorption tank. Therefore, the to-be-processed gas containing the high concentration organic solvent can be introduced into the first adsorption tank. The concentration of the organic solvent in the gas to be treated supplied to the first adsorption tank is preferably 5000 ppm or more, more preferably 10,000 to 100,000 ppm. By setting the concentration of the organic solvent in the gas to be treated to 5000 ppm or more, the saturated adsorption amount of the organic solvent to the ACF becomes 30% or more according to the graph of FIG. That is, the removal process can be performed while maintaining a high adsorption amount.
　この操作だけを考えれば、ＡＣＦを充填した第１吸着槽は、従来の有機溶剤処理方法と比較して、２倍のＡＣＦの吸着量を引き出す事が出来ることになる。 Considering only this operation, the first adsorption tank filled with ACF can draw out the adsorption amount of ACF twice as much as that of the conventional organic solvent treatment method.
　このことは、ＡＣＦの充填量を半分に減らすことができると表現することもできる。この場合は、設備費が半減することは当然ながら、ＡＣＦを再生するユーティリティーも半減することになる。 This can also be expressed as reducing the ACF filling amount in half. In this case, as a matter of course, the facility cost is halved, and the utility for regenerating the ACF is also halved.
　具体的には、第１吸着槽中のＡＣＦ充填量と、第２吸着槽中のＡＣＦ充填量との合計量は、１槽のみを用いる従来の有機溶剤吸着槽中のＡＣＦ充填量と比較して、５２．５～６２．５質量％、少なくとも６０～６２．５質量％に低減する。 Specifically, the total amount of the ACF filling amount in the first adsorption tank and the ACF filling amount in the second adsorption tank is compared with the ACF filling amount in the conventional organic solvent adsorption tank using only one tank. To 52.5 to 62.5% by mass, and at least 60 to 62.5% by mass.
　このＡＣＦ充填量の低減に比例して、ＡＣＦの再生に必要なエネルギーも低減する。
本発明の有機溶剤の除去方法において、被処理ガス中に含まれる有機溶剤は、特に限定されるものではない。本発明の有機溶剤の除去方法は、低沸点の有機溶剤の除去方法として好ましく用いることが出来る。本発明で言う低沸点の有機溶剤とは、沸点が１００℃以下、好ましくは沸点が３０～７０℃の有機溶剤である。沸点が３０～７０℃の有機溶剤としては、塩化メチレン、クロロホルム、1,1-ジクロロエチレン等のハロゲン化炭化水素系有機溶剤、メチラール、メチル-t-ブチルエーテル等のエーテル又はアセタール系有機溶剤、酢酸メチル、酢酸エチル等のエステル系有機溶剤、アセトン、メチルエチルケトン等のケトン系有機溶剤などが挙げられる。 In proportion to the reduction of the ACF filling amount, the energy required for ACF regeneration is also reduced.
In the organic solvent removal method of the present invention, the organic solvent contained in the gas to be treated is not particularly limited. The method for removing an organic solvent of the present invention can be preferably used as a method for removing an organic solvent having a low boiling point. The low-boiling organic solvent referred to in the present invention is an organic solvent having a boiling point of 100 ° C. or lower, preferably 30 to 70 ° C. Examples of organic solvents having a boiling point of 30 to 70 ° C. include halogenated hydrocarbon organic solvents such as methylene chloride, chloroform and 1,1-dichloroethylene, ethers such as methylal and methyl-t-butyl ether, or acetal organic solvents, and methyl acetate. And ester organic solvents such as ethyl acetate, and ketone organic solvents such as acetone and methyl ethyl ketone.
　本発明の有機溶剤の除去装置によれば、第１吸着槽と、第２吸着槽とを連結する連結管には凝縮器が介装され、これにより第１吸着槽処理ガスの中の水分量が低減されているので、第２吸着槽の脱着処理後のＡＣＦを乾燥させるのに、有利なものになっている。凝縮器の入口と出口とにおける第１吸着槽処理ガスの温度降下は、１５～３５℃が好ましく、２０～３５℃が更に好ましい。凝縮器により、第１吸着槽処理ガスの中の水分量の３５～６５％が除去される。 According to the organic solvent removing apparatus of the present invention, a condenser is interposed in the connecting pipe connecting the first adsorption tank and the second adsorption tank, whereby the amount of water in the first adsorption tank treatment gas is increased. This is advantageous for drying the ACF after the desorption treatment of the second adsorption tank. The temperature drop of the first adsorption tank processing gas at the inlet and outlet of the condenser is preferably 15 to 35 ° C, more preferably 20 to 35 ° C. The condenser removes 35 to 65% of the water content in the first adsorption tank processing gas.
　また、第１吸着槽に充填されるＡＣＦと、第２吸着槽に充填されるＡＣＦとの質量比を上述の範囲にすることで、第２吸着槽に導入される第１吸着槽処理ガスの流量は、脱着処理後の第２吸着槽のＡＣＦを乾燥させるのに充分な流量となる。よって、第２吸着槽においては、脱着処理後、従来の方法のように乾燥工程を独立して設ける必要がない。吸着工程において、第１吸着槽処理ガスにより、第２吸着槽のＡＣＦが速やかに乾燥され、効率よく溶剤除去を行うことができる。 In addition, by setting the mass ratio of the ACF filled in the first adsorption tank and the ACF filled in the second adsorption tank to the above range, the first adsorption tank treatment gas introduced into the second adsorption tank The flow rate is sufficient to dry the ACF in the second adsorption tank after the desorption process. Therefore, in the second adsorption tank, it is not necessary to provide a drying step independently after the desorption treatment as in the conventional method. In the adsorption step, the ACF in the second adsorption tank is quickly dried by the first adsorption tank treatment gas, and the solvent can be efficiently removed.
　本発明の有機溶剤の除去方法は、第1吸着槽に導入される被処理ガスの流量によらず、好適に用いることが出来る。特に、第1吸着槽に導入される被処理ガスの流量が比較的小流量である場合にも、好適に用いることが出来る。本発明で言う被処理ガスが比較的小流量である場合とは、被処理ガスの流量が、吸着剤1kgに対して1.0Nm3/min以下の場合を言う。本発明の有機溶剤の処理方法は、被処理ガスの流量が吸着剤1kgに対して1.0Nm3/min　以下、中でも0.2～0.6Nm3/minの場合に特に優れた効果を発揮する。 The method for removing an organic solvent of the present invention can be preferably used regardless of the flow rate of the gas to be treated introduced into the first adsorption tank. In particular, it can be suitably used even when the flow rate of the gas to be treated introduced into the first adsorption tank is relatively small. The case where the gas to be treated is a relatively small flow rate in the present invention refers to a case where the flow rate of the gas to be treated is 1.0 Nm 3 / min or less with respect to 1 kg of the adsorbent. The method for treating an organic solvent of the present invention exhibits particularly excellent effects when the flow rate of the gas to be treated is 1.0 Nm 3 / min or less, particularly 0.2 to 0.6 Nm 3 / min, per 1 kg of the adsorbent.
　第１吸着槽のＡＣＦの質量(Ｍ１)と第２吸着槽のＡＣＦの質量(Ｍ２)との質量比(Ｍ２／Ｍ１)が０．０５未満の場合は、第２吸着槽において有機溶剤の吸着処理が不充分になり、第２吸着槽処理ガス中に含まれる有機溶剤の濃度が高くなるので好ましくない。 When the mass ratio (M 2 / M 1 ) between the mass (M 1 ) of the ACF in the first adsorption tank and the mass (M 2 ) of the ACF in the second adsorption tank is less than 0.05, This is not preferable because the organic solvent adsorption treatment becomes insufficient and the concentration of the organic solvent contained in the second adsorption tank treatment gas becomes high.
　第１吸着槽のＡＣＦの質量(Ｍ１)と第２吸着槽のＡＣＦの質量(Ｍ２)との質量比(Ｍ２／Ｍ１)が０．２５を超える場合は、第２吸着槽のＡＣＦの乾燥に必要な第１吸着槽処理ガス流量が不足する。その結果、第２吸着槽のＡＣＦが乾燥不足になり、第２吸着槽のＡＣＦが水分過多状態になる。このＡＣＦは、吸着効率が低下しているので、第２吸着槽から排出される処理ガス(処理済ガス)に含まれる有機溶剤の含有量が増加する。 When the mass ratio (M 2 / M 1 ) between the mass (M 1 ) of the ACF in the first adsorption tank and the mass (M 2 ) of the ACF in the second adsorption tank exceeds 0.25, The first adsorption tank processing gas flow rate required for drying the ACF is insufficient. As a result, the ACF in the second adsorption tank becomes insufficiently dried, and the ACF in the second adsorption tank becomes in an excessive water state. Since this ACF has reduced adsorption efficiency, the content of the organic solvent contained in the processing gas (treated gas) discharged from the second adsorption tank increases.
　以上のように、本発明の有機溶剤の除去方法及び装置は、吸着材であるＡＣＦの利用効率を高め、ＡＣＦの使用量を軽減し、惹いては装置を小型化するという目的を実現するものである。 As described above, the method and apparatus for removing an organic solvent of the present invention realizes the purpose of increasing the use efficiency of ACF as an adsorbent, reducing the amount of ACF used, and eventually reducing the size of the apparatus. It is.
　次いで、本発明の形態を説明する。 Next, embodiments of the present invention will be described.
  図２は本発明の有機溶剤の除去装置の一例を示すシステムフロー図である。本発明の有機溶剤の除去装置は、大別すると、下記第１吸着槽(Ａ)と、第２吸着槽（Ｂ）とから構成される吸着除去手段系列を有する。
(Ａ)：有機溶剤をＡＣＦに吸着させ及びＡＣＦから脱着させる処理をバッチ処理で行い、この処理により被処理ガスから有機溶剤を分離除去する第１吸着槽
(Ｂ)：前記第１吸着槽で処理済のガス(第１吸着槽処理ガス)中に含まれる有機溶剤をＡＣＦに吸着させ及びＡＣＦから脱着させる処理をバッチ処理で行う第２吸着槽 FIG. 2 is a system flow diagram showing an example of the organic solvent removing apparatus of the present invention. The organic solvent removing apparatus of the present invention is broadly classified into a series of adsorption removing means composed of the following first adsorption tank (A) and second adsorption tank (B).
(A): A first adsorption tank in which an organic solvent is adsorbed on and desorbed from the ACF by batch treatment, and the organic solvent is separated and removed from the gas to be treated by this treatment.
(B): a second adsorption tank in which the organic solvent contained in the gas treated in the first adsorption tank (first adsorption tank treatment gas) is adsorbed on the ACF and desorbed from the ACF by a batch process.
　図２に示すように、本例の有機溶剤の除去装置においては、有機化合物の吸着除去操作が可能な吸着除去手段系列を二系列設ける。一方の吸着除去手段系列(第１吸着槽Ａ、第２吸着槽Ｂ)においては、有機化合物を吸着させる操作を行う。その間、他方の吸着除去手段系列(第１吸着槽Ａ’、第２吸着槽Ｂ’)においては、吸着された有機化合物を脱着させて除去する操作を行う。一方の系列の吸着除去能力が予め設定された限度以下になると、一方の吸着除去手段系列において、吸着された有機化合物を脱着させて除去する操作を行う。同時に、その間、他方の吸着除去手段系列において、有機化合物を吸着させる操作を行う。これらの吸着する操作と、脱着させる操作とは、交互に行う。 As shown in FIG. 2, in the organic solvent removal apparatus of this example, two adsorption removal means series capable of adsorption removal of organic compounds are provided. In one adsorption removal means series (the first adsorption tank A and the second adsorption tank B), an operation for adsorbing an organic compound is performed. Meanwhile, in the other adsorption removal means series (first adsorption tank A ′, second adsorption tank B ′), an operation of desorbing and removing the adsorbed organic compound is performed. When the adsorption removal capability of one series falls below a preset limit, an operation of desorbing and removing the adsorbed organic compound is performed in one adsorption removal means series. At the same time, an operation for adsorbing the organic compound is performed in the other adsorption removal means series. These adsorbing operations and desorbing operations are alternately performed.
　一方の吸着除去手段系列(第１吸着槽Ａ、第２吸着槽Ｂ)と、他方の吸着除去手段系列(第１吸着槽Ａ’、第２吸着槽Ｂ’)とは、その機能は実質的に同一である。同様に、各系列間において、それぞれが有する機械要素も実質的に同一である。したがって、以下の説明においては、同一の機能を果たす機械要素に関しては、ダッシュ記号(’)を付すことで、両系列を互いに区別する。 The function of one adsorption removal means series (first adsorption tank A, second adsorption tank B) and the other adsorption removal means series (first adsorption tank A ′, second adsorption tank B ′) is substantially the same. Are identical. Similarly, machine elements included in each series are substantially the same. Therefore, in the following description, with respect to machine elements that perform the same function, both series are distinguished from each other by adding a dash (').
　図２に示されるように、有機溶剤を５０００ｐｐｍ以上、好ましくは１００００～１０００００ｐｐｍ含有する被処理ガスは、ブロワ２により第１吸着槽導入ライン４を搬送されて、第１吸着槽ＡにおけるＡＣＦ６を充填した第１吸着槽主体８へ導入される。この様な被処理ガスとしては、工場、作業場で発生する排出ガス等が例示される。被処理ガスの温度としては、１０～７０℃が好ましく、２０～５０℃がより好ましい。 As shown in FIG. 2, the gas to be treated containing an organic solvent of 5000 ppm or more, preferably 10,000 to 100,000 ppm is transported by the blower 2 through the first adsorption tank introduction line 4 and filled with ACF 6 in the first adsorption tank A. The first adsorption tank main body 8 is introduced. Examples of such gas to be treated include exhaust gas generated in factories and workplaces. The temperature of the gas to be treated is preferably 10 to 70 ° C, more preferably 20 to 50 ° C.
　第１吸着槽主体８は、塔頂、筒底を閉塞された円筒状の吸着槽と、その内部に挿入された円筒状のＡＣＦ６を有する。第１吸着槽主体８の下部側には、低壁を通してスチーム注入手段１５がＡＣＦ６内に挿入されている。脱着工程においては、このスチーム注入手段１５を通して、スチームがＡＣＦ６の中空部内に供給される。スチームが、ＡＣＦ６の中心から外方に向けて、ＡＣＦ６中を透過する際に、ＡＣＦ６に吸着している有機溶剤の脱着が行われる。 The first adsorption tank main body 8 has a cylindrical adsorption tank with the tower top and the cylinder bottom closed, and a cylindrical ACF 6 inserted therein. A steam injection means 15 is inserted into the ACF 6 through a low wall on the lower side of the first adsorption tank main body 8. In the desorption process, steam is supplied into the hollow portion of the ACF 6 through the steam injection means 15. When the steam permeates through the ACF 6 from the center of the ACF 6 to the outside, the organic solvent adsorbed on the ACF 6 is desorbed.
　ＡＣＦ６の吸着能力は、ＡＣＦ１ｇに対する有機溶剤の吸着量で０．０５～０．５ｇが好ましく、０．１～０．４ｇがより好ましい。ＡＣＦの比表面積は、１２００～２０００ｍ２／ｇが好ましく、１４００～２０００ｍ２／ｇがより好ましく、１４５０～１６００ｍ２／ｇが特に好ましい。 The adsorption capacity of ACF6 is preferably 0.05 to 0.5 g, more preferably 0.1 to 0.4 g in terms of the amount of organic solvent adsorbed on 1 g of ACF. The specific surface area of the ACF is preferably 1200 ~ 2000m 2 / g, more preferably 1400 ~ 2000m 2 / g, particularly preferably 1450 ~ 1600m 2 / g.
　図１によれば、被処理ガスの有機溶剤濃度が１０００ｐｐｍ以上の場合には、比表面積が大きいＡＣＦの吸着量が比表面積が小さいＡＣＦの吸着量よりも高くなる。従って、被処理ガスの有機溶剤濃度が１０００ｐｐｍ以上の場合、比表面積が１２００ｍ２／ｇ以上のＡＣＦ６を使用することが好ましい。更に、比表面積が１２００ｍ２／ｇ以上のＡＣＦ６は、従来の溶剤除去装置では除去できなかった、高分子量の有機化合物も捕集することができる。但し、比表面積が２０００ｍ２／ｇを超えるＡＣＦ６は、平均細孔径が大きいので、溶剤分子と細孔の相互作用が弱くなる。その結果、溶剤の捕集が不十分になる傾向がある。 According to FIG. 1, when the concentration of the organic solvent in the gas to be treated is 1000 ppm or more, the adsorption amount of ACF having a large specific surface area is higher than the adsorption amount of ACF having a small specific surface area. Therefore, when the organic solvent concentration of the gas to be treated is 1000 ppm or more, it is preferable to use ACF6 having a specific surface area of 1200 m 2 / g or more. Furthermore, ACF6 having a specific surface area of 1200 m 2 / g or more can also collect high molecular weight organic compounds that could not be removed by conventional solvent removal apparatuses. However, since ACF6 having a specific surface area exceeding 2000 m 2 / g has a large average pore diameter, the interaction between the solvent molecules and the pores is weakened. As a result, solvent collection tends to be insufficient.
　第１吸着槽ＡにおけるＡＣＦ６の吸着量は、ＡＣＦ６の平均細孔直径及び全細孔容積と、相関性が高い。従って、ＡＣＦ６は、平均細孔直径が１～４ｎｍの範囲にあることが好ましく、３～４ｎｍのものが更に好ましい。また、ＡＣＦ６は、全細孔容積が０．２～０．８ｃｍ３／ｇのものが好ましく、０．３～０．６ｃｍ３／ｇのものがより好ましく、０．５～０．６ｃｍ３／ｇのものが特に好ましい。 The amount of ACF6 adsorbed in the first adsorption tank A is highly correlated with the average pore diameter and total pore volume of ACF6. Therefore, ACF6 preferably has an average pore diameter in the range of 1 to 4 nm, more preferably 3 to 4 nm. Moreover, ACF 6 is preferably one of the total pore volume of 0.2 ~ 0.8cm 3 / g, more preferably those of 0.3 ~ 0.6cm 3 / g, 0.5 ~ 0.6cm 3 / Particularly preferred is g.
　本発明で使用するＡＣＦ６及び後述のＡＣＦ２６としては、吸着するべき有機溶剤の物性を勘案し、該有機溶剤の吸着に適した平均細孔直径、全細孔容積、比表面積を持つＡＣＦを選択することが好ましい。ＡＣＦとしては、ポリアクリロニトリル(ＰＡＮ)系、ピッチ系、セルロース系及びフェノール系など、にんいのＡＣＦが使用できる。これらＡＣＦのうち、フェノール系ＡＣＦは、比表面積が大きくなるほど、平均細孔直径が大きくなる。従って、比表面積の大きいフェノール系ＡＣＦを採用する場合は、細孔を閉塞すること無く、またＡＣＦの吸着性能低下を起すことなく、分子径の大きな高分子化合物も吸着、脱着が可能となる。 As the ACF 6 used in the present invention and the ACF 26 described later, an ACF having an average pore diameter, total pore volume, and specific surface area suitable for adsorption of the organic solvent is selected in consideration of the physical properties of the organic solvent to be adsorbed. It is preferable. As the ACF, garlic ACFs such as polyacrylonitrile (PAN), pitch, cellulose, and phenol can be used. Among these ACFs, the average pore diameter of the phenolic ACF increases as the specific surface area increases. Therefore, when a phenol-based ACF having a large specific surface area is employed, a polymer compound having a large molecular diameter can be adsorbed and desorbed without clogging the pores and without lowering the adsorption performance of ACF.
　第１吸着槽主体８は、吸着除去手段系列数に応じて、１槽以上の複数槽(本例では２槽)配置される。 The first adsorption tank main body 8 is arranged in a plurality of one tank or more (two tanks in this example) according to the number of adsorption removal means series.
　例えば、第１吸着槽主体８が２槽配置される本例の場合は、吸入バルブ１０、１０’及び排出バルブ１２、１２’の交互の切替え、及び蒸気バルブ１４、１４’の交互の切替えにより、絶えず、何れかの第１吸着槽主体８、８’において、吸着工程又は脱着工程が交互に行われる。 For example, in the case of this example in which two first adsorption tank main bodies 8 are arranged, by alternately switching the suction valves 10, 10 ′ and the discharge valves 12, 12 ′ and alternately switching the steam valves 14, 14 ′. The adsorption process or the desorption process is alternately performed in any one of the first adsorption tank main bodies 8 and 8 ′.
　以下、主として、一方の系列の、第１吸着槽Ａについて説明する。 Hereinafter, the first adsorption tank A of one series will be mainly described.
　脱着工程において、第１吸着槽Ａにスチームを供給し、ＡＣＦ６を加熱することにより、ＡＣＦ６から有機溶剤を脱着する脱着工程を行った後に、吸着工程に移行する。吸着工程においては、吸着工程の開始に先立ち、冷却、乾燥用ガスを用いてＡＣＦ６の冷却及び乾燥処理を行なわなくても良い。ＡＣＦ６は、ミクロポアがＡＣＦの外部表面に存在するため、有機溶剤含有ガスを被処理ガスとしてＡＣＦ６に導入するだけで、ＡＣＦ６の冷却及び乾燥が進行し、その吸着活性が徐々に高まる。 In the desorption process, steam is supplied to the first adsorption tank A, and the ACF 6 is heated to perform the desorption process of desorbing the organic solvent from the ACF 6, and then the process proceeds to the adsorption process. In the adsorption process, it is not necessary to cool and dry the ACF 6 using the cooling and drying gas prior to the start of the adsorption process. Since ACF6 has micropores on the outer surface of the ACF, simply introducing an organic solvent-containing gas into the ACF6 as a gas to be processed advances the cooling and drying of the ACF6 and gradually increases its adsorption activity.
　後述する吸着工程において第１吸着槽主体８内のＡＣＦ６には、有機溶剤が吸着されている。この有機溶剤は、脱着工程において、第１吸着槽主体８へスチームを導入することにより脱着され、ＡＣＦ６が再生され、同時に有機溶剤含有第１吸着槽脱着ガスが第１吸着槽主体８外部に取出される。スチームは、第１吸着槽側スチーム導入ライン１６、蒸気バルブ１４、スチーム注入手段１５を通じて、第１吸着槽主体８内に注入される。なお、再生されたＡＣＦ６は、前記注入されたスチームが凝縮した水分を含む湿潤状態にある。 In the adsorption process described later, an organic solvent is adsorbed on the ACF 6 in the first adsorption tank main body 8. In the desorption process, the organic solvent is desorbed by introducing steam into the first adsorption tank main body 8 to regenerate the ACF 6 and at the same time, the organic solvent-containing first adsorption tank desorption gas is taken out of the first adsorption tank main body 8. Is done. Steam is injected into the first adsorption tank main body 8 through the first adsorption tank side steam introduction line 16, the steam valve 14, and the steam injection means 15. Note that the regenerated ACF 6 is in a wet state containing moisture condensed from the injected steam.
　有機溶剤含有第１吸着槽脱着ガスは、第１吸着槽側脱着ガスバルブ１８、第１吸着槽側回収ライン２０を通って後述の有機溶剤含有第２吸着槽脱着ガスと共に凝縮器２２へ導入される。有機溶剤含有第１吸着槽脱着ガスは、凝縮器２２において冷却水により冷却される。この凝縮処理により、凝縮分として回収有機溶剤が得られる。他方、未凝縮分は、被処理ガスに混入される(図２)。 The organic solvent-containing first adsorption tank desorption gas passes through the first adsorption tank-side desorption gas valve 18 and the first adsorption tank-side recovery line 20 and is introduced into the condenser 22 together with the organic solvent-containing second adsorption tank desorption gas described later. . The organic solvent-containing first adsorption tank desorption gas is cooled by cooling water in the condenser 22. By this condensation treatment, a recovered organic solvent is obtained as a condensed component. On the other hand, the uncondensed component is mixed into the gas to be processed (FIG. 2).
　吸着工程においては、被処理ガスは、ブロア２により第１吸着槽導入ライン４を通して、第１吸着槽Ａに送られる。被処理ガスは、ここでＡＣＦ６により有機溶剤の吸着が行われ、同時に第１吸着槽処理ガスが第１吸着槽Ａから外部に取出される。第１吸着槽Ａから排出される第１吸着槽処理ガス中の有機溶剤濃度は好ましくは１０～１０００ｐｐｍ、より好ましくは１００～２００ｐｐｍになるように、運転条件を選定する。取出される第１吸着槽処理ガスの温度は、通常３０～７０℃である。 In the adsorption process, the gas to be treated is sent to the first adsorption tank A through the first adsorption tank introduction line 4 by the blower 2. The gas to be treated is adsorbed with the organic solvent by the ACF 6 and the first adsorption tank processing gas is taken out from the first adsorption tank A to the outside at the same time. The operating conditions are selected so that the concentration of the organic solvent in the first adsorption tank treatment gas discharged from the first adsorption tank A is preferably 10 to 1000 ppm, more preferably 100 to 200 ppm. The temperature of the first adsorption tank processing gas taken out is usually 30 to 70 ° C.
　この第１吸着槽処理ガスは、第１吸着槽と第２吸着槽とを連結するパイプからなる第１吸着槽処理ガス輸送ライン２４を通って、凝縮器２５に送られる。 The first adsorption tank processing gas is sent to the condenser 25 through the first adsorption tank processing gas transport line 24 composed of a pipe connecting the first adsorption tank and the second adsorption tank.
　第１吸着槽処理ガスは、前記脱着工程で注入したスチームが凝縮して湿潤状態にあるＡＣＦ６を乾燥させる際に生成する水分を飽和状態近くまで含む。この水分を含む第１吸着槽処理ガスは、凝縮器２５において、スチームに由来する蒸気を凝縮分離された後、第２吸着槽Ｂに送られる。 The first adsorption tank treatment gas contains moisture generated when the steam injected in the desorption step is condensed to dry the ACF 6 in a wet state to near saturation. The first adsorption tank processing gas containing moisture is sent to the second adsorption tank B after the vapor derived from steam is condensed and separated in the condenser 25.
　凝縮器２５で凝縮分離される水分量は、第１吸着槽処理ガスに含まれる全水分量の少なくとも３０質量％以上が好ましい。凝縮器の入口と出口とにおける第１吸着槽処理ガスの温度降下を１５～３５℃に保つことにより、第１吸着槽処理ガス中の水分量の３５～６５％を除去できる。 The amount of water condensed and separated by the condenser 25 is preferably at least 30% by mass or more of the total amount of water contained in the first adsorption tank processing gas. By maintaining the temperature drop of the first adsorption tank processing gas at the inlet and outlet of the condenser at 15 to 35 ° C., 35 to 65% of the moisture content in the first adsorption tank processing gas can be removed.
　上記吸着工程における吸着処理により、第１吸着槽処理ガス中の有機溶剤濃度は、５００ｐｐｍ以下になる。 The organic solvent concentration in the first adsorption tank treatment gas becomes 500 ppm or less by the adsorption treatment in the adsorption step.
　第２吸着槽Ｂにおいては、第１吸着槽処理ガス中に残存する有機溶剤がＡＣＦ２６により吸着除去されると共に、有機溶剤濃度が低下された第２吸着槽処理ガスが外部に排出される。 In the second adsorption tank B, the organic solvent remaining in the first adsorption tank processing gas is removed by adsorption by the ACF 26, and the second adsorption tank processing gas having a reduced organic solvent concentration is discharged to the outside.
　第２吸着槽主体２８は、第１吸着槽主体８と同様に、系列数に応じて１槽、又は複数槽(本例では２槽)配置されている。例えば、本例の２槽の場合は、吸入バルブ３０、３０’及び排出バルブ３２、３２’の交互の切替え、及び蒸気バルブ３４、３４’の交互の切替えにより、第２吸着槽主体２８、２８’ の何れかにおいて、吸着又は脱着が交互に行われる。第２吸着槽Ｂの構成は、第１吸着槽Ａの構成とほぼ同一である。 As with the first adsorption tank main body 8, the second adsorption tank main body 28 is arranged in one tank or a plurality of tanks (two tanks in this example) according to the number of series. For example, in the case of the two tanks of this example, the second adsorption tank main bodies 28, 28 are obtained by alternately switching the suction valves 30, 30 ′ and the discharge valves 32, 32 ′ and alternately switching the steam valves 34, 34 ′. 'Adsorption or desorption takes place alternately in any of the soots. The configuration of the second adsorption tank B is substantially the same as the configuration of the first adsorption tank A.
　以下、主として、一方の系列の第２吸着槽Ｂについて説明する。 Hereinafter, the second adsorption tank B of one series will be mainly described.
　ＡＣＦ２６は、ＡＣＦ１ｇに対する有機溶剤の吸着量が０．０５～０．５ｇ、好ましくは０．１～０．４ｇが好ましい。ＡＣＦ２６の比表面積は、６００ｍ２／ｇ以上１４００ｍ２／ｇ未満が好ましく、７００ｍ２／ｇ以上１４００ｍ２／ｇ未満がより好ましく、１１００～１３５０ｍ２／ｇが更に好ましく、１２００～１３５０ｍ２／ｇが特に好ましい。 ACF26 has an organic solvent adsorption amount of 1 to ACF of 0.05 to 0.5 g, preferably 0.1 to 0.4 g. The specific surface area of ACF26 is preferably less than 600 meters 2 / g or more 1400 m 2 / g, more preferably less than 700 meters 2 / g or more 1400 m 2 / g, more preferably 1100 ~ 1350m 2 / g, 1200 ~ 1350m 2 / g is Particularly preferred.
　また、ＡＣＦ２６の平均細孔直径は０．５～３ｎｍが好ましく、平均細孔直径が１～２．５ｎｍがより好ましい。全細孔容積は、０．１～０．６ｃｍ３／ｇが好ましく、０．２～０．４ｃｍ３／ｇがより好ましい。 The average pore diameter of ACF26 is preferably 0.5 to 3 nm, and the average pore diameter is more preferably 1 to 2.5 nm. Total pore volume is preferably 0.1 ~ 0.6cm 3 / g, more preferably 0.2 ~ 0.4cm 3 / g.
　上記ＡＣＦ６とＡＣＦ２６との組合せを採用することにより、前述のように、ＡＣＦの吸着能力を最大限発揮させる事が出来る。 By adopting a combination of the above ACF6 and ACF26, the adsorption capacity of ACF can be maximized as described above.
　第２吸着槽主体２８に吸着される有機溶剤は、脱着工程において、第２吸着槽主体２８へスチームを導入することにより脱着される。スチームは、第２吸着槽側スチーム導入ライン３６、蒸気バルブ３４、スチーム注入手段３５を通って、第２吸着槽主体２８に送られる。このスチームにより、ＡＣＦ２６が再生され、同時に有機溶剤含有第２吸着槽脱着ガスが生成する。この有機溶剤含有第２吸着槽脱着ガスは、第２吸着槽側脱着ガスバルブ３８、第２吸着槽側回収ライン４０を通って、前述の有機溶剤含有第１吸着槽脱着ガスと共に凝縮器２２へ導入送られる。有機溶剤含有第２吸着槽脱着ガスは、凝縮器２２において、冷却水で冷却する凝縮処理が行われる。この凝集処理により、凝縮分として回収有機溶剤が得られる。未凝縮分は、被処理ガスに混入された後、第１吸着槽に送られる。(図２)。 The organic solvent adsorbed on the second adsorption tank main body 28 is desorbed by introducing steam into the second adsorption tank main body 28 in the desorption step. The steam is sent to the second adsorption tank main body 28 through the second adsorption tank side steam introduction line 36, the steam valve 34, and the steam injection means 35. By this steam, the ACF 26 is regenerated, and simultaneously, an organic solvent-containing second adsorption tank desorption gas is generated. The organic solvent-containing second adsorption tank desorption gas is introduced into the condenser 22 together with the organic solvent-containing first adsorption tank desorption gas through the second adsorption tank-side desorption gas valve 38 and the second adsorption tank-side recovery line 40. Sent. In the condenser 22, the organic solvent-containing second adsorption tank desorption gas is subjected to a condensation process of cooling with cooling water. By this aggregation treatment, a recovered organic solvent is obtained as a condensed component. The uncondensed component is mixed into the gas to be treated and then sent to the first adsorption tank. (Figure 2).
　吸着工程においては、系外に排出される第２吸着槽処理ガス（清浄化ガス）中の有機溶剤濃度は、１００ｐｐｍ以下、好ましくは６０ｐｐｍ以下、更に好ましくは３０ｐｐｍ以下に制御される。 In the adsorption step, the concentration of the organic solvent in the second adsorption tank processing gas (cleaning gas) discharged out of the system is controlled to 100 ppm or less, preferably 60 ppm or less, more preferably 30 ppm or less.
　必要に応じ、第２吸着槽処理ガスを、バックアップ処理槽(不図示)に導入して、更に有機溶剤濃度を低減させても良い。バックアップ処理槽は、第２吸着槽処理ガス輸送ライン４２に接続すればよい。 If necessary, the second adsorption tank processing gas may be introduced into a backup processing tank (not shown) to further reduce the organic solvent concentration. The backup processing tank may be connected to the second adsorption tank processing gas transport line 42.
　バックアップ処理槽としては、特に制限がないが、吸着材を担持した耐熱紙等を多数の通路を有するハニカム状に加工した回転ドラム型有機溶剤処理装置が挙げられる（特開平９－３０８８１４号）。バックアップ処理槽に担持される吸着材としては、ＡＣＦ、ゼオライトなどが挙げられる。 The backup treatment tank is not particularly limited, and examples thereof include a rotating drum type organic solvent treatment apparatus in which heat-resistant paper carrying an adsorbent is processed into a honeycomb shape having a large number of passages (Japanese Patent Laid-Open No. 9-308814). Examples of the adsorbent supported in the backup processing tank include ACF and zeolite.
　図２の例においては、２つの凝縮器２５、２５’を設けている。しかし、この例に限られず、図３の例のように、１つの凝縮器２５を、吸着工程と脱着工程との切換時に、切換えて使用するようにしても良い。図３の例の場合は、設備コストが低減できる。 In the example of FIG. 2, two condensers 25 and 25 'are provided. However, the present invention is not limited to this example, and one condenser 25 may be used by switching at the time of switching between the adsorption process and the desorption process as in the example of FIG. In the case of the example of FIG. 3, the equipment cost can be reduced.
　以下、実施例により本発明を更に具体的に説明するが、本発明はこれら実施例に限定されるものではない。 Hereinafter, the present invention will be described more specifically by way of examples. However, the present invention is not limited to these examples.
　ＡＣＦの比表面積、平均細孔直径及び全細孔容積は、全自動ガス吸着量測定装置(Quantachrome Instruments社製ＡＵＴＯＳＯＲＢ－１)を用いて、以下に記載した条件で測定した。
吸着ガス：窒素
吸着温度：液体窒素温度(－１９６℃)
測定範囲：Ｐ／Ｐ０＝０．００～０．９９
比表面積は、得られた吸着等温線からＢＥＴ法を用いて算出した。全細孔容積は、相対圧１．０近傍の吸着量の液体換算により算出した。平均細孔直径は、全細孔容積と比表面積から、下式(１) 
平均細孔直径＝４×全細孔容積÷比表面積・・・(１)
を用いて算出した。 The specific surface area, average pore diameter and total pore volume of ACF were measured under the conditions described below using a fully automatic gas adsorption amount measuring device (AUTOSORB-1 manufactured by Quantachrome Instruments).
Adsorption gas: Nitrogen adsorption temperature: Liquid nitrogen temperature (-196 ° C)
Measurement range: P / P 0 = 0.00 to 0.99
The specific surface area was calculated from the obtained adsorption isotherm using the BET method. The total pore volume was calculated by liquid conversion of the amount of adsorption near the relative pressure of 1.0. The average pore diameter is calculated from the following formula (1) from the total pore volume and specific surface area.
Average pore diameter = 4 × total pore volume / specific surface area (1)
It calculated using.
　［実施例１］
　図３に示す２系列の除去装置を用いて被処理ガス中の有機溶剤を除去した。処理条件を表１及び下記に示した。 [Example 1]
The organic solvent in the gas to be treated was removed using two series of removal apparatuses shown in FIG. The processing conditions are shown in Table 1 and below.
　有機溶剤として、２００００ｐｐｍの塩化メチレン(沸点４０℃)を含有する被処理ガスを、３Ｎｍ３／ｍｉｎで８分間吸着工程を行った。吸着工程後、ＡＣＦ６及び２６に、温度１２０℃のＡＣＦ再生用蒸気量１３ｋｇ／ｈを６分間供給し、ＡＣＦ６、２６の脱着工程を行った。上記の吸着・脱着工程を交互に行うことで、被処理ガスを連続的に除去処理した。 A gas to be treated containing 20000 ppm of methylene chloride (boiling point: 40 ° C.) as an organic solvent was subjected to an adsorption step at 3 Nm 3 / min for 8 minutes. After the adsorption process, the ACF regeneration steam amount of 13 kg / h at a temperature of 120 ° C. was supplied to the ACFs 6 and 26 for 6 minutes, and the desorption process of the ACFs 6 and 26 was performed. The gas to be treated was continuously removed by alternately performing the adsorption / desorption steps described above.
　第１吸着槽Ａにおいて用いたＡＣＦ６は、充填質量(Ｍ１)が５ｋｇ、比表面積が１５００ｍ２／ｇ、平均細孔直径が１．５ｎｍ、全細孔容積が０．５５ｃｍ３／ｇであった。 The ACF 6 used in the first adsorption tank A had a packed mass (M 1 ) of 5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.5 nm, and a total pore volume of 0.55 cm 3 / g. It was.
　第２吸着槽Ｂにおいて用いたＡＣＦ２６は、充填質量(Ｍ２)が０．５ｋｇ、比表面積が１３００ｍ２／ｇ、平均細孔直径が０．５ｎｍ、全細孔容積が０．３ｃｍ３／ｇであった。第１吸着槽Ａと第２吸着槽ＢとのＡＣＦ充填質量比(Ｍ２／Ｍ１)は０．１であった。なお、ＡＣＦ６及び２６はフェノール系ＡＣＦ(東邦化工建設社製)を円筒状に形成したものであった。 The ACF 26 used in the second adsorption tank B has a filling mass (M 2 ) of 0.5 kg, a specific surface area of 1300 m 2 / g, an average pore diameter of 0.5 nm, and a total pore volume of 0.3 cm 3 / g. Met. The ACF filling mass ratio (M 2 / M 1 ) between the first adsorption tank A and the second adsorption tank B was 0.1. ACFs 6 and 26 were phenolic ACFs (Toho Kako Construction Co., Ltd.) formed in a cylindrical shape.
　第１吸着槽Ａと、第２吸着槽Ｂとを連結する連結管２４に介装された凝縮器２５における入口と出口の温度降下は、２０℃に設定した。 The temperature drop at the inlet and the outlet of the condenser 25 interposed in the connecting pipe 24 connecting the first adsorption tank A and the second adsorption tank B was set to 20 ° C.
　この吸脱着処理において、吸着処理開始後１ｈｒの第１吸着槽処理ガス中の塩化メチレン濃度(処理済ガス濃度)と、吸着処理開始から１ｈｒ経過するまでの期間に排出された有機溶剤の総量(有機溶剤排出量)と、ＡＣＦ再生用蒸気量の測定結果を表１に示す。 In this adsorption / desorption treatment, the methylene chloride concentration (treated gas concentration) in the first adsorption tank treatment gas for 1 hr after the start of the adsorption treatment, and the total amount of organic solvent discharged in the period from the start of the adsorption treatment to 1 hr ( Table 1 shows the measurement results of the amount of organic solvent discharged) and the amount of steam for ACF regeneration.
　結果は、第２吸着槽処理ガス(処理済ガス)中の有機溶剤の濃度は１０ｐｐｍと低く、塩化メチレン排出量も７ｇ／ｈと低いものであった。ＡＣＦの再生に使用した蒸気量は２５ｋｇ／ｈと少なく、脱着処理は効率の良いものであった。 As a result, the concentration of the organic solvent in the second adsorption tank treatment gas (treated gas) was as low as 10 ppm, and the methylene chloride discharge was as low as 7 g / h. The amount of steam used for ACF regeneration was as low as 25 kg / h, and the desorption treatment was efficient.
　［実施例２］
表１に示すように、ＡＣＦ２６の比表面積を１５００ｍ２／ｇ、平均細孔直径を１．５ｎｍ、全細孔容積を０．５５ｃｍ３／ｇにした以外は、実施例１と同様に操作した。 [Example 2]
As shown in Table 1, the same operation as in Example 1 was performed except that the specific surface area of ACF26 was 1500 m 2 / g, the average pore diameter was 1.5 nm, and the total pore volume was 0.55 cm 3 / g. .
　結果は、処理済ガス中の塩化メチレン濃度は５０ｐｐｍと低く、塩化メチレン排出量も３５ｇ／ｈと低いものであった。 As a result, the methylene chloride concentration in the treated gas was as low as 50 ppm, and the methylene chloride discharge was as low as 35 g / h.
　また、ＡＣＦ再生用蒸気量は２５ｋｇ／ｈと少なく、脱着処理は効率の良いものであった。 Moreover, the amount of steam for ACF regeneration was as low as 25 kg / h, and the desorption treatment was efficient.
　［実施例３］
表１に示すように、ＡＣＦ６及び２６としてピッチ系ＡＣＦ(東邦化工建設社製)を用いた以外は、実施例１と同様に操作した。 [Example 3]
As shown in Table 1, operations were performed in the same manner as in Example 1 except that pitch-type ACF (manufactured by Toho Kako Construction Co., Ltd.) was used as ACFs 6 and 26.
　第１吸着槽Ａにおいて用いたＡＣＦ６は、充填質量(Ｍ１)が５ｋｇ、比表面積が１５００ｍ２／ｇ、平均細孔直径が１．３ｎｍ、全細孔容積が０．５ｃｍ３／ｇのピッチ系ＡＣＦであった。第２吸着槽Ｂにおいて用いたＡＣＦ２６は、充填質量(Ｍ２)が０．５ｋｇ、比表面積が１５００ｍ２／ｇ、平均細孔直径が１．３ｎｍ、全細孔容積が０．５ｃｍ３／ｇのピッチ系ＡＣＦであった。第１吸着槽Ａと第２吸着槽ＢとのＡＣＦ充填質量比(Ｍ２／Ｍ１)は０．１であった。 The ACF 6 used in the first adsorption tank A has a pitch with a packing mass (M 1 ) of 5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.3 nm, and a total pore volume of 0.5 cm 3 / g. System ACF. The ACF 26 used in the second adsorption tank B has a filling mass (M 2 ) of 0.5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.3 nm, and a total pore volume of 0.5 cm 3 / g. The pitch ACF. The ACF filling mass ratio (M 2 / M 1 ) between the first adsorption tank A and the second adsorption tank B was 0.1.
　吸脱着処理の結果は、処理済ガス中の塩化メチレン濃度は５０ｐｐｍと低く、塩化メチレン排出量も３５ｇ／ｈと低いものであった。 As a result of the adsorption / desorption treatment, the methylene chloride concentration in the treated gas was as low as 50 ppm, and the methylene chloride discharge was as low as 35 g / h.
　また、ＡＣＦ再生用蒸気量は２７ｋｇ／ｈと少なく、脱着処理は効率の良いものであった。 Further, the amount of steam for ACF regeneration was as small as 27 kg / h, and the desorption treatment was efficient.
　［実施例４］
  表１に示すように、ＡＣＦ６及び２６として、ＰＡＮ系ＡＣＦ(東邦化工建設社製)を用いた以外は、実施例１と同様に操作した。 [Example 4]
As shown in Table 1, the same operation as in Example 1 was performed except that PAN-based ACF (manufactured by Toho Kako Construction Co., Ltd.) was used as ACFs 6 and 26.
　第１吸着槽Ａにおいて用いたＡＣＦ６は、充填質量(Ｍ１)が５ｋｇ、比表面積が１５００ｍ２／ｇ、平均細孔直径が１．３ｎｍ、全細孔容積が０．５ｃｍ３／ｇであった。第２吸着槽Ｂにおいて用いたＡＣＦ２６は、充填質量(Ｍ２)が０．５ｋｇ、比表面積が１５００ｍ２／ｇ、平均細孔直径が１．３ｎｍ、全細孔容積が０．５ｃｍ３／ｇであった。第１吸着槽Ａと第２吸着槽ＢとのＡＣＦ充填質量比(Ｍ２／Ｍ１)は０．１であった。 The ACF 6 used in the first adsorption tank A had a packed mass (M 1 ) of 5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.3 nm, and a total pore volume of 0.5 cm 3 / g. It was. The ACF 26 used in the second adsorption tank B has a filling mass (M 2 ) of 0.5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.3 nm, and a total pore volume of 0.5 cm 3 / g. Met. The ACF filling mass ratio (M 2 / M 1 ) between the first adsorption tank A and the second adsorption tank B was 0.1.
　吸脱着処理の結果は、処理済ガス中の塩化メチレン濃度が８０ｐｐｍと低く、塩化メチレン排出量が５６ｇ／ｈと低いものであった。 The results of the adsorption / desorption treatment were such that the methylene chloride concentration in the treated gas was as low as 80 ppm and the methylene chloride discharge was as low as 56 g / h.
　ＡＣＦ再生用蒸気量は２９ｋｇ／ｈと少なく、脱着処理は効率の良いものであった。 The amount of steam for ACF regeneration was as low as 29 kg / h, and the desorption treatment was efficient.
　［実施例５］
表１に示すように、ＡＣＦ６にフェノール系ＡＣＦ(東邦化工建設社製)を用い、ＡＣＦ２６にＰＡＮ系ＡＣＦ(東邦化工建設社製)を用いた以外は、実施例１と同様に操作した。
第１吸着槽Ａにおいて用いたＡＣＦ６は、充填質量(Ｍ１)が５ｋｇ、比表面積が１５００ｍ２／ｇ、平均細孔直径が１．５ｎｍ、全細孔容積が０．５５ｃｍ３／ｇのフェノール系ＡＣＦであった。第２吸着槽Ｂにおいて用いたＡＣＦ２６は、充填質量(Ｍ２)が０．５ｋｇ、比表面積が１５００ｍ２／ｇ、平均細孔直径が１．３ｎｍ、全細孔容積が０．５ｃｍ３／ｇのＰＡＮ系ＡＣＦであった。第１槽Ａと第２吸着槽ＢとのＡＣＦ充填質量比(Ｍ２／Ｍ１)は０．１であった。 [Example 5]
As shown in Table 1, the same operation as in Example 1 was performed except that phenol-based ACF (manufactured by Toho Kako Construction Co.) was used for ACF6 and PAN-based ACF (manufactured by Toho Kako Construction Co.) was used for ACF26.
The ACF 6 used in the first adsorption tank A is a phenol having a filling mass (M 1 ) of 5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.5 nm, and a total pore volume of 0.55 cm 3 / g. System ACF. The ACF 26 used in the second adsorption tank B has a filling mass (M 2 ) of 0.5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.3 nm, and a total pore volume of 0.5 cm 3 / g. PAN-based ACF. The ACF filling mass ratio (M 2 / M 1 ) between the first tank A and the second adsorption tank B was 0.1.
　吸脱着処理の結果は、処理済ガス中の塩化メチレン濃度は８０ｐｐｍと低く、塩化メチレン排出量も５６ｇ／ｈと低いものであった。 As a result of the adsorption / desorption treatment, the methylene chloride concentration in the treated gas was as low as 80 ppm, and the methylene chloride discharge was as low as 56 g / h.
　また、ＡＣＦ再生用蒸気量は２７ｋｇ／ｈと少なく、脱着処理は効率の良いものであった。 Further, the amount of steam for ACF regeneration was as small as 27 kg / h, and the desorption treatment was efficient.
Figure JPOXMLDOC01-appb-T000001
Figure JPOXMLDOC01-appb-T000001
　［比較例１］
　表２に示すように、ＡＣＦを充填した吸着槽として１槽のみを用いて、吸脱着処理した以外は、実施例１と同様に操作した。 [Comparative Example 1]
As shown in Table 2, the same operation as in Example 1 was carried out except that only one tank was used as the adsorption tank filled with ACF and the adsorption / desorption treatment was performed.
　有機溶剤吸着槽において用いたＡＣＦは、充填質量が５．５ｋｇ、比表面積が１５００ｍ２／ｇ、平均細孔直径が１．５ｎｍ、全細孔容積が０．５５ｃｍ３／ｇであった。 The ACF used in the organic solvent adsorption tank had a filling mass of 5.5 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.5 nm, and a total pore volume of 0.55 cm 3 / g.
　吸脱着処理の結果、処理済ガス中の塩化メチレン濃度は２００ｐｐｍと高くなり、塩化メチレン排出量も１４０ｇ／ｈと高いものとなった。 As a result of the adsorption / desorption treatment, the methylene chloride concentration in the treated gas was as high as 200 ppm, and the methylene chloride discharge was as high as 140 g / h.
　また、ＡＣＦ再生用蒸気量は３３ｋｇ／ｈと多く、脱着処理は効率の悪いものであった。 Moreover, the amount of steam for ACF regeneration was as high as 33 kg / h, and the desorption treatment was inefficient.
　［実施例６］
　表２に示すように、被処理ガス中の塩化メチレン濃度を５００００ｐｐｍとした以外は、実施例１と同様に操作した。 [Example 6]
As shown in Table 2, the same operation as in Example 1 was performed except that the concentration of methylene chloride in the gas to be treated was changed to 50000 ppm.
　吸脱着処理の結果は、処理済ガス中の塩化メチレン濃度は２０ｐｐｍと低く、塩化メチレン排出量も７ｇ／ｈと低いものであった。 As a result of the adsorption / desorption treatment, the methylene chloride concentration in the treated gas was as low as 20 ppm, and the methylene chloride discharge was as low as 7 g / h.
　また、ＡＣＦ再生用蒸気量は２５ｋｇ／ｈと少なく、脱着処理は効率の良いものであった。
［比較例２］
　表２に示すように、ＡＣＦを充填した吸着槽１槽のみで、吸脱着処理した以外は、実施例６と同様に操作した。 Further, the amount of steam for ACF regeneration was as low as 25 kg / h, and the desorption treatment was efficient.
[Comparative Example 2]
As shown in Table 2, the same operation as in Example 6 was carried out except that only one adsorption tank filled with ACF was subjected to the adsorption / desorption treatment.
　有機溶剤吸着槽において用いたＡＣＦは、充填質量が８ｋｇ、比表面積が１５００ｍ２／ｇ、平均細孔直径が１．５ｎｍ、全細孔容積が０．５５ｃｍ３／ｇであった。 The ACF used in the organic solvent adsorption tank had a packed mass of 8 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.5 nm, and a total pore volume of 0.55 cm 3 / g.
　吸脱着処理の結果は、実施例６に比べ多量のＡＣＦを使用しているにも拘らず、処理済ガス中の塩化メチレン濃度は５００ｐｐｍと高くなり、塩化メチレン排出量も１７５ｇ／ｈと高いものとなった。 As a result of the adsorption / desorption treatment, the methylene chloride concentration in the treated gas was as high as 500 ppm and the methylene chloride discharge was as high as 175 g / h, although a large amount of ACF was used as compared with Example 6. It became.
　また、ＡＣＦ再生用蒸気量は３３ｋｇ／ｈと多く、脱着処理は効率の悪いものであった。 Moreover, the amount of steam for ACF regeneration was as high as 33 kg / h, and the desorption treatment was inefficient.
　［実施例７］
  表２に示すように、有機溶剤として２００００ｐｐｍのクロロホルム(沸点６１℃)を含有する被処理ガスを用いた以外は、実施例１と同様に操作した。 [Example 7]
As shown in Table 2, the same operation as in Example 1 was performed except that a gas to be treated containing 20000 ppm of chloroform (boiling point 61 ° C.) was used as the organic solvent.
　吸脱着処理の結果は、処理済ガス中のクロロホルム濃度は５０ｐｐｍと低く、クロロホルム排出量も２８ｇ／ｈと低いものであった。 As a result of the adsorption / desorption treatment, the chloroform concentration in the treated gas was as low as 50 ppm, and the chloroform discharge was as low as 28 g / h.
　また、ＡＣＦ再生用蒸気量は２５ｋｇ／ｈと少なく、脱着処理は効率の良いものであった。 Moreover, the amount of steam for ACF regeneration was as low as 25 kg / h, and the desorption treatment was efficient.
　［比較例３］
　表２に示すように、ＡＣＦを充填した吸着槽１槽のみで、吸脱着処理した以外は、実施例７と同様に操作した。 [Comparative Example 3]
As shown in Table 2, the same operation as in Example 7 was carried out except that only one adsorption tank filled with ACF was subjected to the adsorption / desorption treatment.
　有機溶剤吸着槽において用いたＡＣＦは、充填質量が８ｋｇ、比表面積が１５００ｍ２／ｇ、平均細孔直径が１．５ｎｍ、全細孔容積が０．５５ｃｍ３／ｇであった。 The ACF used in the organic solvent adsorption tank had a packed mass of 8 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.5 nm, and a total pore volume of 0.55 cm 3 / g.
　吸脱着処理の結果は、実施例７と比較して多量のＡＣＦを使用しているにも拘らず、処理済ガス中のクロロホルム濃度は３００ｐｐｍと高くなり、クロロホルム排出量も１７０ｇ／ｈと高いものとなった。 As a result of the adsorption / desorption treatment, the chloroform concentration in the treated gas was as high as 300 ppm and the chloroform discharge amount was as high as 170 g / h, even though a large amount of ACF was used as compared with Example 7. It became.
　また、ＡＣＦ再生用蒸気量は３３ｋｇ／ｈと多く、脱着処理は効率の悪いものであった。 Moreover, the amount of steam for ACF regeneration was as high as 33 kg / h, and the desorption treatment was inefficient.
Figure JPOXMLDOC01-appb-T000002
Figure JPOXMLDOC01-appb-T000002
［実施例８］
　表３に示すように、被処理ガス流量を２２０Ｎｍ３／ｈとした。被処理ガスの流量増加に伴い、ＡＣＦ充填量を第１吸着槽Ａ(Ｍ１)が６ｋｇ、第２吸着槽Ｂ(Ｍ２)が０．６ｋｇとした以外は、実施例１と同様に操作した。第１槽Ａと、第２槽ＢとのＡＣＦ充填質量比(Ｍ２／Ｍ１)が０．１、全体(Ｍ１＋Ｍ２)が６．６ｋｇであった。 [Example 8]
As shown in Table 3, the gas flow rate to be treated was 220 Nm 3 / h. The same operation as in Example 1 was performed except that the ACF filling amount was set to 6 kg for the first adsorption tank A (M 1 ) and 0.6 kg for the second adsorption tank B (M 2 ) as the gas flow increased. did. The ACF filling mass ratio (M 2 / M 1 ) between the first tank A and the second tank B was 0.1, and the whole (M 1 + M 2 ) was 6.6 kg.
　吸脱着処理の結果は、処理済ガス中の塩化メチレン濃度が１０ｐｐｍで低く、塩化メチレン排出量も１０ｇ／ｈと低いものであった。 As a result of the adsorption / desorption treatment, the methylene chloride concentration in the treated gas was as low as 10 ppm, and the methylene chloride discharge was as low as 10 g / h.
　ＡＣＦ再生用蒸気量は２９ｋｇ／ｈであった。実施例１と比較すると、使用したＡＣＦ量の増加に伴い、ＡＣＦ再生用蒸気量は増加しているが、脱着処理効率は十分に良いものであった。
［比較例４］
　表３に示すように、ＡＣＦを充填した吸着槽１槽のみで、吸脱着処理した以外は、実施例８と同様に操作した。 The amount of steam for ACF regeneration was 29 kg / h. Compared to Example 1, the amount of steam for ACF regeneration increased as the amount of ACF used increased, but the desorption efficiency was sufficiently good.
[Comparative Example 4]
As shown in Table 3, the same operation as in Example 8 was performed except that only one adsorption tank filled with ACF was subjected to the adsorption / desorption treatment.
　有機溶剤吸着槽において用いたＡＣＦは、充填質量が１２ｋｇ、比表面積が１５００ｍ２／ｇ、平均細孔直径が１．５ｎｍ、全細孔容積が０．５５ｃｍ３／ｇであった。 The ACF used in the organic solvent adsorption tank had a filling mass of 12 kg, a specific surface area of 1500 m 2 / g, an average pore diameter of 1.5 nm, and a total pore volume of 0.55 cm 3 / g.
　本比較例においては、１２ｋｇの大量のＡＣＦを使用した。しかし、処理済ガス中の塩化メチレン濃度は３００ｐｐｍと高くなり、塩化メチレン排出量も３００ｇ／ｈと高かった。 In this comparative example, a large amount of 12 kg of ACF was used. However, the methylene chloride concentration in the treated gas was as high as 300 ppm, and the methylene chloride discharge was as high as 300 g / h.
　また、ＡＣＦ再生用蒸気量は５２ｋｇ／ｈと多く、脱着処理は効率の悪いものであった。 Also, the amount of steam for ACF regeneration was as high as 52 kg / h, and the desorption treatment was inefficient.
Figure JPOXMLDOC01-appb-T000003
Figure JPOXMLDOC01-appb-T000003
［施例９］
　表４に示すように、ＡＣＦ充填量を第１吸着槽Ａ(Ｍ１)が５ｋｇ、第２吸着槽Ｂ(Ｍ２)が０．３ｋｇとした以外は、実施例１と同様に操作した。第１吸着槽Ａと、第２吸着槽ＢとのＡＣＦ充填質量比(Ｍ２／Ｍ１)は０．０６、全体(Ｍ１＋Ｍ２)は５．３ｋｇであった。 [Example 9]
As shown in Table 4, the same operation as in Example 1 was performed except that the ACF filling amount was 5 kg for the first adsorption tank A (M 1 ) and 0.3 kg for the second adsorption tank B (M 2 ). The ACF filling mass ratio (M 2 / M 1 ) between the first adsorption tank A and the second adsorption tank B was 0.06, and the whole (M 1 + M 2 ) was 5.3 kg.
　吸脱着処理の結果は、処理済ガス中の塩化メチレン濃度は１０ｐｐｍと低く、塩化メチレン排出量も７ｇ／ｈと低いものであった。 As a result of the adsorption / desorption treatment, the methylene chloride concentration in the treated gas was as low as 10 ppm, and the methylene chloride discharge was as low as 7 g / h.
　また、ＡＣＦ再生用蒸気量は２３ｋｇ／ｈであり、脱着処理は効率の良いものであった。 Also, the amount of steam for ACF regeneration was 23 kg / h, and the desorption treatment was efficient.
　［比較例５］
　表４に示すように、ＡＣＦ充填量を第１吸着槽Ａ(Ｍ１)が５ｋｇ、第２吸着槽Ｂ(Ｍ２)が０．２ｋｇとした以外は、実施例１と同様に操作した。第１吸着槽Ａと、第２吸着槽ＢとのＡＣＦ充填質量比(Ｍ２／Ｍ１)は０．０４、全体(Ｍ１＋Ｍ２)は５．２ｋｇであった。 [Comparative Example 5]
As shown in Table 4, the same operation as in Example 1 was performed except that the ACF filling amount was 5 kg for the first adsorption tank A (M 1 ) and 0.2 kg for the second adsorption tank B (M 2 ). The ACF filling mass ratio (M 2 / M 1 ) between the first adsorption tank A and the second adsorption tank B was 0.04, and the whole (M 1 + M 2 ) was 5.2 kg.
　吸脱着処理の結果は、処理済ガス中の塩化メチレン濃度は１５０ｐｐｍと高かった。塩化メチレン排出量は１０５ｇ／ｈで、高かった。 As a result of the adsorption / desorption treatment, the methylene chloride concentration in the treated gas was as high as 150 ppm. The methylene chloride discharge was high at 105 g / h.
　［実施例１０］
　表４に示すように、ＡＣＦ充填量を第１吸着槽Ａ(Ｍ１)が５ｋｇ、第２吸着槽Ｂ(Ｍ２)が１ｋｇとした以外は、実施例１と同様に操作した。第１吸着槽Ａと、第２吸着槽ＢとのＡＣＦ充填質量比(Ｍ２／Ｍ１)は０．２、全体(Ｍ１＋Ｍ２)は６ｋｇであった。 [Example 10]
As shown in Table 4, the same operation as in Example 1 was performed except that the ACF filling amount was 5 kg for the first adsorption tank A (M 1 ) and 1 kg for the second adsorption tank B (M 2 ). The ACF filling mass ratio (M 2 / M 1 ) between the first adsorption tank A and the second adsorption tank B was 0.2, and the whole (M 1 + M 2 ) was 6 kg.
　吸脱着試験の結果は、処理済ガス中の塩化メチレン濃度は２０ｐｐｍと低く、塩化メチレン排出量も１４ｇ／ｈと低いものであった。 As a result of the adsorption / desorption test, the methylene chloride concentration in the treated gas was as low as 20 ppm, and the methylene chloride discharge was as low as 14 g / h.
　また、ＡＣＦ再生用蒸気量は２４ｋｇ／ｈと少なく、脱着処理は効率の良いものであった。 Also, the amount of steam for ACF regeneration was as low as 24 kg / h, and the desorption treatment was efficient.
　［比較例６］
　表４に示すように、ＡＣＦ充填量を第１吸着槽Ａ(Ｍ１)が４．５ｋｇ、第２吸着槽Ｂ(Ｍ２)が１．５ｋｇとした以外は、実施例１と同様に操作した。第１吸着槽Ａと、第２吸着槽ＢとのＡＣＦ充填質量比(Ｍ２／Ｍ１)は０．３３３、全体(Ｍ１＋Ｍ２)は６ｋｇであった。 [Comparative Example 6]
As shown in Table 4, the same operation as in Example 1 was performed except that the ACF filling amount was 4.5 kg for the first adsorption tank A (M 1 ) and 1.5 kg for the second adsorption tank B (M 2 ). did. The ACF filling mass ratio (M 2 / M 1 ) between the first adsorption tank A and the second adsorption tank B was 0.333, and the whole (M 1 + M 2 ) was 6 kg.
　吸脱着処理の結果は、ＡＣＦ再生用蒸気量は２３ｋｇ／ｈと少なく、脱着処理は効率の良いものではあった。しかし、第２吸着槽Ｂの乾燥が不充分になり、その結果、処理済ガス中の塩化メチレン濃度は１５０ｐｐｍと高くなった。塩化メチレン排出量も１０５ｇ／ｈと高かった。 As a result of the adsorption / desorption treatment, the amount of steam for ACF regeneration was as small as 23 kg / h, and the desorption treatment was efficient. However, the drying of the second adsorption tank B became insufficient, and as a result, the methylene chloride concentration in the treated gas was as high as 150 ppm. The methylene chloride discharge was as high as 105 g / h.
Figure JPOXMLDOC01-appb-T000004
Figure JPOXMLDOC01-appb-T000004
　［実施例１１］
　表２及び下記の条件に示すように、有機溶剤として２００００ｐｐｍのメチラール(沸点４２．５℃)]を含有する被処理ガスを用いた以外は、実施例１と同様に操作した。 [Example 11]
As shown in Table 2 and the following conditions, the same operation as in Example 1 was performed except that a gas to be treated containing 20000 ppm methylal (boiling point 42.5 ° C.) as an organic solvent was used.
　この吸脱着試験の結果、処理済ガス中のメチラール濃度は８０ｐｐｍと低く、メチラール排出量も４９ｇ／ｈと低いものであった。 As a result of this adsorption / desorption test, the methylal concentration in the treated gas was as low as 80 ppm, and the methylal discharge was as low as 49 g / h.
　また、ＡＣＦ再生用蒸気量は２９ｋｇ／ｈであり、脱着処理は効率の良いものであった。 Further, the amount of steam for ACF regeneration was 29 kg / h, and the desorption treatment was efficient.
　［実施例１２］
　表２及び下記の条件に示すように、有機溶剤として２００００ｐｐｍの酢酸メチル(沸点５４℃)を含有する被処理ガスを用いた以外は、実施例１と同様に操作した。 [Example 12]
As shown in Table 2 and the following conditions, the same operation as in Example 1 was performed except that a gas to be treated containing 20000 ppm of methyl acetate (boiling point 54 ° C.) was used as the organic solvent.
　この吸脱着試験の結果、処理済ガス中の酢酸メチル濃度は８０ｐｐｍと低く、酢酸メチル排出量も４８ｇ／ｈと低いものであった。 As a result of this adsorption / desorption test, the methyl acetate concentration in the treated gas was as low as 80 ppm and the methyl acetate discharge was as low as 48 g / h.
　また、ＡＣＦ再生用蒸気量は２８ｋｇ／ｈと少なく、脱着処理は効率の良いものであった。 Moreover, the amount of steam for ACF regeneration was as small as 28 kg / h, and the desorption treatment was efficient.
　［実施例１３］
　表５に示すように、有機溶剤として２００００ｐｐｍのアセトン(沸点５６．５℃)を含有する被処理ガスを用いた以外は、実施例１と同様に操作した。 [Example 13]
As shown in Table 5, the same operation as in Example 1 was performed except that a gas to be treated containing 20000 ppm of acetone (boiling point: 56.5 ° C.) was used as the organic solvent.
　吸脱着処理の結果は、処理済ガス中のアセトン濃度は５０ｐｐｍと低く、アセトン排出量も２４ｇ／ｈと低いものであった。 As a result of the adsorption / desorption treatment, the concentration of acetone in the treated gas was as low as 50 ppm, and the amount of acetone discharged was as low as 24 g / h.
　また、ＡＣＦ再生用蒸気量は２８ｋｇ／ｈと少なく、脱着処理は効率の良いものであった。 Moreover, the amount of steam for ACF regeneration was as small as 28 kg / h, and the desorption treatment was efficient.
Figure JPOXMLDOC01-appb-T000005
Figure JPOXMLDOC01-appb-T000005

Claims (6)

  1. 活性炭素繊維が充填される第１吸着槽と、
    　前記活性炭素繊維と同一又は異なる活性炭素繊維が充填される第２吸着槽であって、第２吸着槽に充填される活性炭素繊維の質量(Ｍ２)が、第１吸着槽に充填される活性炭素繊維の質量(Ｍ１)を基準として、質量比(Ｍ２／Ｍ１)で０．０５～０．２５である第２吸着槽と、
    　前記第１吸着槽と、第２吸着槽とを連結する連結管と、
    　前記連結管に介装される凝縮器と、
    　前記第１吸着槽及び第２吸着槽にそれぞれ設けられるスチーム注入手段と、
    　を有する有機溶剤の除去装置。     A first adsorption tank filled with activated carbon fibers;
    The second adsorption tank filled with activated carbon fibers that are the same as or different from the activated carbon fibers, and the mass (M 2 ) of activated carbon fibers filled in the second adsorption tank is filled in the first adsorption tank. A second adsorption tank having a mass ratio (M 2 / M 1 ) of 0.05 to 0.25 on the basis of the mass (M 1 ) of the activated carbon fiber;
    A connecting pipe connecting the first adsorption tank and the second adsorption tank;
    A condenser interposed in the connecting pipe;
    Steam injection means provided in each of the first adsorption tank and the second adsorption tank;
    An organic solvent removing apparatus having
  2. 第１吸着槽に充填される活性炭素繊維が、比表面積１２００ｍ２／ｇ～２０００ｍ２／ｇ、平均細孔直径１～４ｎｍ、全細孔容積０．２～０．８ｃｍ３／ｇの活性炭素繊維である請求の範囲第１項に記載の有機溶剤の除去装置。 The activated carbon fiber filled in the first adsorption tank is activated carbon having a specific surface area of 1200 m 2 / g to 2000 m 2 / g, an average pore diameter of 1 to 4 nm, and a total pore volume of 0.2 to 0.8 cm 3 / g. The organic solvent removing apparatus according to claim 1, which is a fiber.
  3. 第２吸着槽に充填される活性炭素繊維が、比表面積６００ｍ２／ｇ以上１４００ｍ２／ｇ未満、平均細孔直径０．５～３ｎｍ、全細孔容積０．１～０．６ｃｍ３／ｇの活性炭素繊維である請求の範囲第１項に記載の有機溶剤の除去装置。 The activated carbon fiber filled in the second adsorption tank has a specific surface area of 600 m 2 / g or more and less than 1400 m 2 / g, an average pore diameter of 0.5 to 3 nm, and a total pore volume of 0.1 to 0.6 cm 3 / g. The organic solvent removing apparatus according to claim 1, which is an activated carbon fiber.
  4. 請求の範囲第１項に記載の有機溶剤の除去装置を用いる被処理ガス中の有機溶剤の除去方法であって、
    　有機溶剤を３０００ｐｐｍ以上含む被処理ガスを第１吸着槽に供給してその内部に充填される活性炭素繊維に有機溶剤を吸着させると共に、活性炭素繊維に含まれる凝縮水の乾燥を行うことにより、水分と５００ｐｐｍ以下の有機溶剤とを含む第１吸着槽処理ガスを得、次いでこの第１吸着槽処理ガスを凝縮器に供給して第１吸着槽処理ガス中の水分を凝縮分離して系外に排出すると共に、前記水分を分離した第１吸着槽処理ガスを第２吸着槽に供給して、第２吸着槽の内部に充填される活性炭素繊維に第１吸着槽処理ガスが含む有機溶剤を吸着させると共に、この活性炭素繊維が含む水分を乾燥させることにより、有機溶剤濃度が１００ｐｐｍ以下の第２吸着槽処理ガスを系外に排出させる吸着工程と、
    　第１吸着槽に供給する被処理ガスの供給を停止した後、スチーム注入手段により第１吸着槽及び第２吸着槽内にスチームを供給して、第１吸着槽及び第２吸着槽内に充填されている各活性炭素繊維が吸着している有機溶剤を脱着させることにより、前記有機溶剤を吸着している各活性炭素繊維を、前記供給したスチームが凝縮して生じる凝縮水を含む活性炭素繊維に、再生させると共に、前記脱着させた有機溶剤を系外に取出す脱着工程と、
    　を交互に繰返す被処理ガス中の有機溶剤の除去方法。     A method for removing an organic solvent in a gas to be treated using the organic solvent removing apparatus according to claim 1,
    By supplying the gas to be treated containing 3000 ppm or more of the organic solvent to the first adsorption tank and adsorbing the organic solvent to the activated carbon fiber filled therein, and drying the condensed water contained in the activated carbon fiber, A first adsorption tank treatment gas containing moisture and an organic solvent of 500 ppm or less is obtained, and then the first adsorption tank treatment gas is supplied to a condenser to condense and separate the moisture in the first adsorption tank treatment gas. And the first adsorption tank processing gas from which the moisture has been separated is supplied to the second adsorption tank, and the activated carbon fiber filled in the second adsorption tank contains the organic solvent contained in the first adsorption tank processing gas. An adsorption step of discharging the second adsorption tank processing gas having an organic solvent concentration of 100 ppm or less to the outside by drying the moisture contained in the activated carbon fiber.
    After the supply of the gas to be processed to be supplied to the first adsorption tank is stopped, steam is supplied into the first adsorption tank and the second adsorption tank by the steam injection means, and the first adsorption tank and the second adsorption tank are filled. Activated carbon fibers containing condensed water produced by the condensation of the supplied steam by desorbing the organic solvent adsorbed by each activated carbon fiber being adsorbed to each activated carbon fiber adsorbing the organic solvent And a desorption step of regenerating and taking out the desorbed organic solvent out of the system,
    The method of removing the organic solvent in the gas to be processed that repeats alternately.
  5. 凝縮器の入口と出口とにおける第１吸着槽処理ガスの温度降下を１５～３５℃に保つことにより、第１吸着槽処理ガス中の水分量の３５～６５％を除去する請求の範囲第４項に記載の有機溶剤の除去方法。 Claim 4 wherein 35 to 65% of the moisture content in the first adsorption tank process gas is removed by maintaining the temperature drop of the first adsorption tank process gas at the inlet and outlet of the condenser at 15 to 35 ° C. The method for removing the organic solvent according to item.
  6. 第１吸着槽に供給する被処理ガスが、沸点が３０～７０℃の有機溶剤を５０００～１０００００ｐｐｍ含む被処理ガスである請求の範囲第４項に記載の有機溶剤の除去方法。 The method for removing an organic solvent according to claim 4, wherein the gas to be treated supplied to the first adsorption tank is a gas to be treated containing 5000 to 100,000 ppm of an organic solvent having a boiling point of 30 to 70 ° C.
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