WO2000025900A1 - Procede et dispositif de recuperation de vapeurs d'hydrocarbures - Google Patents

Procede et dispositif de recuperation de vapeurs d'hydrocarbures Download PDF

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Publication number
WO2000025900A1
WO2000025900A1 PCT/JP1999/005899 JP9905899W WO0025900A1 WO 2000025900 A1 WO2000025900 A1 WO 2000025900A1 JP 9905899 W JP9905899 W JP 9905899W WO 0025900 A1 WO0025900 A1 WO 0025900A1
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Prior art keywords
hydrocarbon vapor
gas
hydrocarbon
adsorption
vapor
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PCT/JP1999/005899
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English (en)
Japanese (ja)
Inventor
Yuichi Eto
Shigemi Okanishi
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Idemitsu Engineering Co., Ltd.
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Application filed by Idemitsu Engineering Co., Ltd. filed Critical Idemitsu Engineering Co., Ltd.
Priority to JP2000579332A priority Critical patent/JP3711327B6/ja
Priority to KR1020017005281A priority patent/KR20010085967A/ko
Publication of WO2000025900A1 publication Critical patent/WO2000025900A1/fr

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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
    • 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
    • B01D53/047—Pressure swing adsorption
    • 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
    • B01D2257/702—Hydrocarbons
    • 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
    • B01D2259/40001—Methods relating to additional, e.g. intermediate, treatment of 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
    • B01D2259/402—Further details for adsorption processes and devices using two beds

Definitions

  • the present invention recovers hydrocarbon vapor contained in air and other gases discharged from the storage facility when liquid hydrocarbons such as gasoline are charged into storage facilities such as storage tanks and expansion due to temperature. And a device for performing the method.
  • the following invention has been proposed (JP-A-10-156127).
  • the exhaust gas containing high-concentration benzene is brought into contact with pre-cooled heavy oil or benzene to partially remove the benzene vapor, and then the benzene vapor is removed in the adsorption tower filled with the adsorbent. Adsorption is removed.
  • the pressure is reduced by a vacuum pump or the like while the adsorption tower is heated by a heating coil or the like through which steam flows inside.
  • the separated benzene is returned to the above-mentioned recovery tower, where it is condensed and recovered.
  • the benzene vapor is partially recovered and then adsorbed in the adsorption tower, so that benzene can be removed to near the limit and post-treatment of the separated benzene is easy.
  • the adsorption tower is heated by a heating coil or the like through which steam flows, but this indirect heating method is inefficient.
  • the adsorbent such as silica gel has low thermal conductivity and the granular materials are in point contact with each other, the heat transfer in the adsorbent packed bed is very slow.
  • adsorption PTSA: Pressure & Temporature Swing Adsorption
  • the switching of adsorption and separation is performed in a matter of minutes, but in this time, the temperature rises substantially only to the surface of the heating coil and to a distance of several cm. I can't warm. Therefore, it is necessary to increase the number of heating coils, which requires extra space in the adsorption tower and uneven temperature in the adsorbent layer. The loss of steam for heating was increasing.
  • An object of the present invention is to provide a hydrocarbon vapor recovery method and apparatus capable of efficiently recovering a hydrocarbon vapor from a gas containing a hydrocarbon vapor.
  • a first step of cooling and condensing a gas containing hydrocarbon vapor by a cooling means, and removing a part of the hydrocarbon vapor, and a heating means A second step of heating and raising the temperature of the gas from which a part of the hydrocarbon vapor has been removed, and supplying the heated gas to an adsorption unit filled with an adsorbent; And a third step of adsorbing and removing the one.
  • the temperature of the gas after the treatment in the first step exceeds the freezing point of the contained components and is set to a low temperature near the freezing point of the parentheses.
  • the freezing point of benzene is 5.5 ° C, so it is preferably 6 to 20 ° C, more preferably 6 to 10 ° C. .
  • a first step for example, high-boiling impurities such as toluene, xylene, trimethylbenzene, coumarone, and indene contained in crude gas oil mainly composed of benzene generated by carbonization of coal, especially sublimation Naphthalene, which is a solid, is effectively removed by lowering the vapor pressure by cooling and dissolving in benzene.
  • the temperature of the gas after heating in the second step is preferably 5 to 30 ° C. higher than the temperature after the treatment in the first step. More preferably, the temperature is higher by 10 to 20 ° C.
  • Such a temperature is set because the hydrocarbon vapor has reached the saturated state at the temperature at the time of cooling in the treatment of the first step. If the pressure drops further, condensation or solid precipitation occurs immediately. This phenomenon will cause clogging of pipes, malfunction of switching valves, and increase in pressure loss of adsorption towers.o
  • the temperature of the gas after the first step can be raised, and the degree of saturation of the hydrocarbon vapor can be reduced to prevent condensation in pipes and the like. it can. Further, the temperature of the subsequent adsorption device can be raised to facilitate separation and regeneration after adsorption. Furthermore, the reduction in the concentration of hydrocarbon vapor reduces the load of the next third step, and makes it possible to reduce the size of the adsorption tower and vacuum pump.
  • the temperature of the adsorbent in the adsorption tower rises due to adsorption of hydrocarbon vapor, and falls due to separation.
  • the temperature fluctuation is several ° C. Therefore, immediately after the operation of separating the hydrocarbon vapor from the adsorbent is completed, the gas containing the saturated concentration of the hydrocarbon vapor is discharged immediately after the operation of separating the hydrocarbon vapor from the adsorbent without performing the heating and temperature increasing operation according to the second step. If introduced, it may condense at the inlet of the adsorption tower or solid deposition may occur.
  • silica gel Ordinary adsorbents such as silica gel, alumina gel, and activated carbon can be used. From the viewpoint of safety, use of silica gel, zeolite, or alumina gel is preferred.
  • it is silica gel treated with a high-temperature calcining or hydrophobizing agent or high silica zeolite having a silica / alumina ratio of 80 or more. If the adsorbent adsorbs water in the gas, it is necessary to separate water from the recovered oil, so it is difficult to adsorb water, but a hydrophobic adsorbent that adsorbs hydrocarbons is preferred. It is.
  • the adsorption means is, for example, an adsorption tower.
  • the adsorbent adsorbs and removes the hydrocarbon vapor, and discharges a clean gas.
  • the adsorbent that has adsorbed the hydrocarbons in the third step is regenerated by separating the hydrocarbons by reducing the pressure.
  • the degree of vacuum at the time of separation is preferably 60 Torr or less in absolute pressure. More preferably, the absolute pressure is 25 Torr or less. The lower the absolute pressure, the easier it is for hydrocarbon vapors to separate. If the separation of hydrocarbons is not sufficient, the adsorbent will be less likely to adsorb the hydrocarbon vapor in the next adsorption operation, and the efficiency of removing the hydrocarbon vapor will decrease.
  • the hydrocarbon vapor separated from the adsorbent has a very high concentration and can be easily condensed by cooling and recovered as a liquid.
  • a cooling method a general heat exchanger (tube type, plate type, etc.) can be used.
  • the low-concentration hydrocarbon vapor that could not be condensed can be processed without being discharged out of the apparatus by mixing it with the raw material gas at the entrance of the apparatus.
  • it can be recovered by contacting it with cooled light oil, kerosene, gasoline, recovered oil, etc. to cool and condense it, or dissolving it in these.
  • the low-concentration hydrocarbon vapor that has not been condensed or dissolved may be mixed with the raw material gas at the entrance of the apparatus in the same manner as described above.
  • the separated hydrocarbon vapor may be mixed with a gas containing the hydrocarbon vapor in the first step, and may be cooled and condensed to be recovered.
  • the gas from which the hydrocarbon vapor is to be recovered may be ordinary air, or may be similar to nitrogen or other inert gas, etc., and may be a facility for the production or storage of liquefied hydrocarbons, which are sources of hydrocarbon vapor. It can be applied to various gases and the like discharged from such as appropriate.
  • the condensed liquid hydrocarbon is used, and the cooled liquid hydrocarbon is brought into contact with a gas containing a hydrocarbon vapor to form a hydrocarbon base in the gas. It is desirable to cool and condense the par.
  • the temperature-raised gas from the second step is supplied to the adsorption means to adsorb the hydrocarbon vapor to the adsorbent, and then the pressure in the adsorption means is reduced. Then, it is desirable that a clean gas (normal air or an appropriate gas) be caused to flow back into the adsorption means, and that the hydrocarbons be separated from the adsorbent in this state.
  • a clean gas normal air or an appropriate gas
  • the flow rate of the clean gas which is preferably 1/5 to 1/50, more preferably 1/10 to 50 times the flow rate of the process gas introduced into the adsorption tower during adsorption. 1/20.
  • a plurality of adsorption means are provided, and it is desirable that these adsorption means are alternately switched to an adsorption treatment and a separation treatment to perform a continuous treatment.
  • the switching of the adsorption means is preferably performed within one hour, more preferably within ten minutes. In order to reduce the temperature change of the adsorbent layer by reducing the change in the amount of adsorption of hydrocarbons, short-time switching is preferable.
  • the heat of adsorption is an exotherm, while increasing the temperature makes adsorption more difficult (separation becomes more likely), and conversely, lowering the temperature causes adsorption. Easier (separation is less likely). Therefore, when the hydrocarbon vapor is adsorbed, the temperature of the adsorbent rises, and it becomes difficult to adsorb the hydrocarbon vapor further. Conversely, in the separation operation, when the hydrocarbon vapor separates, the temperature decreases, and further separation of the hydrocarbon vapor becomes difficult. That is, if the adsorption / separation operation is performed, a phenomenon occurs in which the effect of the operation is negated.
  • the hydrocarbon separated from the adsorbent is mixed with the gas containing the hydrocarbon vapor in the first step, and then cooled and condensed to recover.
  • the apparatus for recovering a hydrocarbon vapor comprises: a cooling unit for cooling and condensing a gas containing the hydrocarbon vapor to remove a part of the hydrocarbon vapor; Heating means for heating and raising the temperature of the gas from which a part of the hydrocarbon vapor has been removed; and adsorbing means filled with an adsorbent for adsorbing and removing the hydrocarbon vapor in the heated gas. It is characterized by having.
  • the cooling means is appropriately selected from the following two in accordance with the concentration of the hydrocarbon vapor and the allowable pressure loss.
  • a combination of a normal heat exchanger (tube type, plate type, etc.) and a gas-liquid separator is suitable. If the allowable pressure loss is low, a recovery tower with a built-in heat exchanger or a recovery tower with an external heat exchanger is suitable.
  • This recovery tower has a gas-liquid contact part at the top and a liquid reservoir at the bottom. The lower part is pumped out and introduced into the upper part for circulation.
  • the gas-liquid contact portion is filled with a filler such as a Raschig ring, so that gas-liquid contact can be performed efficiently.
  • the liquid level in the liquid reservoir is controlled by the balance between the pumping amount and the circulation amount.
  • an ordinary heat exchanger such as a tube type or a plate type can be used.
  • a common chiller unit is provided as a supply source of the cooling heat medium supplied to the cooling unit and a supply source of the heating heat medium supplied to the heating unit. .
  • a common chill unit If a common chill unit is used, a single cooling medium and a heating medium can be supplied by one unit, which is economical and advantageous in space.
  • a refrigerator may be used as the cooling unit and the heating unit.
  • a plurality of the adsorbing units are provided so as to alternately switch the adsorption process and the separation process to perform the continuous process.
  • one adsorption tower as the adsorption means may be a single tower, but it is preferable to provide a plurality of adsorption towers and perform the adsorption treatment continuously while switching the adsorption / separation operation.
  • FIG. 1 is a schematic diagram of a hydrocarbon vapor recovery device according to a first embodiment of the present invention.
  • FIG. 2 is a schematic view of a hydrocarbon vapor recovery device according to a second embodiment of the present invention.
  • FIG. 3 is a schematic view of a hydrocarbon vapor recovery device according to a comparative example.
  • FIG. 4 is a schematic view showing a main part of a hydrocarbon vapor recovery apparatus according to another embodiment of the present invention.
  • FIG. 5 is a schematic view showing a main part of a hydrocarbon vapor recovery device according to another embodiment of the present invention.
  • FIG. 6 is a schematic view showing a main part of a hydrocarbon vapor recovery device according to another embodiment of the present invention.
  • the hydrocarbon vapor recovery device of the present embodiment includes a first heat exchanger 11 connected to an introduction line 10 for a gas (here, air) containing hydrocarbon vapor, and a gas supply to the heat exchanger 11.
  • a gas-liquid separator 13 connected via a line 10A
  • a second heat exchanger connected to the gas-liquid separator 13 via a gas supply line 12, and a second heat exchanger 14 Gas supply line with two downstream branches
  • the first and second adsorption towers 15 and 16 connected via the inlet 12A and the gas supply line 33A branched from the vicinity of the adsorption towers 15 and 16 of the gas supply line 12A are connected.
  • the vacuum pump 20 is provided.
  • the first heat exchanger (tube type or plate type) 11 is provided with a refrigerator 17.
  • the gas-liquid separator 13 is provided with a liquid reservoir 19 at a lower portion thereof.
  • a wire mesh type demister (not shown) is installed at the gas outlet of the gas-liquid separator 13.
  • the second heat exchanger (tube type or plate type) 14 is provided with a heater 21.
  • the heating medium of this heat exchanger is hot water.
  • Each of the first and second adsorption towers 15 and 16 has an adsorption layer 22 filled with an adsorbent therein.
  • Each gas supply line 12 from the second heat exchanger 14 to the first and second adsorption towers 15 and 16 is provided with first and second valves 23 and 24.
  • Third and fourth valves 25 and 26 are provided on a gas supply line 33A branched from the gas supply line 12A.
  • the first and second adsorption towers 15 and 16 are each connected at their top to a clean gas discharge line 31, and each line 31 is provided with fifth and sixth valves 27 and 28. I have.
  • a clean gas flows back to the adsorption towers 15 and 16 through a line 31 between the fifth and sixth valves 27 and 28 and the tops of the adsorption towers 15 and 16.
  • a supply line 32 for supplying clean air to be supplied is connected, and each line is provided with seventh and eighth valves 29 and 30.
  • a return line 33 for returning the separated hydrocarbon vapor is provided between the vacuum pump 20 and the introduction line 10 in front of the first heat exchanger 11. The procedure for recovering hydrocarbon vapor using this recovery device is as follows.
  • air containing hydrocarbon vapor is passed through the first heat exchanger 11 from the introduction line 10, where the air is cooled to condense the hydrocarbon vapor,
  • the cooled and condensed hydrocarbons and air are supplied to a gas-liquid separator 13 for gas-liquid separation. Part of the condensed hydrocarbon vapor is collected in the liquid reservoir 19 and collected.
  • the air containing the remaining hydrocarbon vapor is supplied to the second heat exchanger 14 from the outlet.
  • warm water is used as a heat medium, and the air from which a part of the hydrocarbon vapor has been removed is heated to raise the temperature.
  • the heated air is supplied to the first or second adsorption tower 15 or 16, where the hydrocarbon vapor is adsorbed and removed by an adsorbent.
  • first and second adsorption towers 15 and 16 switch the valves 23, 24, 27 and 28 alternately to the adsorption treatment and the separation treatment to continuously process the hydrocarbon vapor.
  • the pressure inside the adsorption towers 15 and 16 is reduced by the vacuum pump 20, and the clean air is flowed back into the adsorption towers 15 and 16 from the clean air supply line 32 to adsorb hydrocarbons in this state. Separate from agent.
  • the hydrocarbon vapor recovery device of the present embodiment includes a recovery tower 36 connected to an introduction line 10 for a gas (here, air) containing hydrocarbon vapor, and a liquid between a lower part and an upper part of the recovery tower 36.
  • a first heat exchanger 11 provided via a hydrocarbon circulation line 39 of the first type, a second heat exchanger 14 connected to the recovery tower 36 via a gas supply line 12, and First and second adsorption towers 15 and 16 connected to the second heat exchanger 14 via a gas supply line 12A whose downstream side is branched into two, and adsorption towers 15 and 16 of these gas supply lines 12A.
  • It is provided with a vacuum pump 20 connected via a gas supply line 33A branched from a portion near 16.
  • the recovery tower 36 is provided with a gas-liquid contact part 37 at the upper part and a liquid reservoir part 38 at the lower part.
  • the gas-liquid contact part 37 is filled with a filler such as a Raschig ring.
  • a wire mesh type demister (not shown) is installed at the gas outlet of the recovery tower 36.
  • One of the liquid hydrocarbon circulation lines 39 is connected to the liquid reservoir 38 side of the recovery tower 36, and the other is inserted above the gas-liquid contact part 37 in the recovery tower 36, and is connected to the end.
  • a liquid hydrocarbon sprayer 41 is provided.
  • a circulation pump 42 is provided between the liquid reservoir 38 of the circulation line 39 and the first heat exchanger 11.
  • Other components of the apparatus for example, the first heat exchanger 11, the second heat exchanger 14, the first and second adsorption towers 15, 16 and the vacuum pump 20, etc. This is the same as the embodiment.
  • the procedure for recovering hydrocarbon vapor using this recovery device is as follows.
  • air containing hydrocarbon vapor is supplied from the introduction line 10 to the recovery tower 36, where the air is cooled to form hydrocarbon vapor.
  • the liquid is condensed and the generated liquid is stored in the liquid reservoir 38.
  • the air is cooled and condensed, the liquid hydrocarbons in the liquid storage section 38 are partially circulated through the circulation line 39 and are cooled in the first heat exchanger 11, and then are collected in the recovery tower 36.
  • the liquid hydrocarbon and the air are brought into contact with each other at a gas-liquid contact section 37 to perform the supply.
  • first heat exchanger 11 is provided with the refrigerator 17 and the second heat exchanger 14 is provided with the heater 21.
  • first heat exchanger 1 A common chiller unit may be provided as a supply source of the cooling heat medium supplied to 1 and a supply source of the heating heat medium supplied to the second heat exchanger 14.
  • the recovery tower 36 may be configured as follows. As shown in FIG. 4, the recovery tower 36 is provided with a gas-liquid disperser 37A such as a chimney tray perforated tray between the gas-liquid contact part 37 and the introduction part of the circulation line 39. A demister 37B is installed above the 39 introduction part. The liquid reservoir 38 is connected to an extraction line 42A extending from the side of the recovery tower 36 to the circulation pump 42, the suction end of which is directed downward, and is arranged radially around it. A vortex breaker 42B made of multiple plates is also installed.
  • a gas-liquid disperser 37A such as a chimney tray perforated tray between the gas-liquid contact part 37 and the introduction part of the circulation line 39.
  • a demister 37B is installed above the 39 introduction part.
  • the liquid reservoir 38 is connected to an extraction line 42A extending from the side of the recovery tower 36 to the circulation pump 42, the suction end of which is directed downward, and is arranged radially around it.
  • the gas-liquid disperser 37A By installing the gas-liquid disperser 37A, further contact between the liquid-phase component returned from the circulation line 39 and the gas-phase component rising through the gas-liquid contact part 37 is achieved. Recovery of liquid phase components can be promoted.
  • the installation of the demist 37B makes it possible to remove mist-like liquid phase components from the gas taken out to the gas supply line 12 at the top of the tower. Further, by installing the vortex breaker 42B, the liquid accumulated in the liquid reservoir 38 from the extraction line 42A is sucked. The occurrence of swirls and gas entrainment on exit is avoided.
  • a structure used in the existing brand technology may be appropriately adopted.
  • a substantially U-shaped recovery tower 36A may be employed.
  • an introduction line 10 is connected to one of the tops (left side in the figure) of a substantially U-shaped recovery tower 36A, and a circulation line 39 is connected slightly below the top.
  • a gas-liquid disperser 37A is installed slightly below the connection part of the circulation line 39, and a gas-liquid contact part 37 is installed below it.
  • the gas supply line 12 is connected to one of the tower tops (right side in the figure), and a demister 37B is installed below it.
  • Such a substantially U-shaped recovery tower 36A also separates the hydrocarbon vapor contained in the gas from the introduction line 10 and the circulation line 39, and supplies the separated gas to the gas supply line. It can be taken out from the line 12 and stored in the liquid reservoir 38.
  • each of the embodiments described above treats a hydrocarbon-containing gas from a single inlet line 10, it may treat hydrocarbon-containing gas from multiple gas sources. In such a case, it is desirable to supplement the structure to avoid mixed contamination (contamination) due to backflow between the gas sources.
  • two introduction lines 10L and 10H are connected to the recovery tower 36A.
  • the introduction line 10L is connected to the top of the tower in the same way as the introduction line 10 in Fig. 5.
  • the introduction line 10H is connected between the gas-liquid contact part 37 of the recovery tower 36A and the gas-liquid disperser 37A.
  • the gas source supplied to the introduction line 10H has a higher concentration or purity of the stored liquid than the gas source supplied to the introduction line 10L.
  • the introduction line 10L is connected to the exhaust port of the crude benzene ink, and the guide line 10H is connected to the exhaust port of the pure benzene ink.
  • the introduction line 10H is simply connected to the recovery tower 36A, the low-purity benzene component from the introduction line 10L is introduced into the recovery tower 36A. Ingredients flow back into the pure benzene tank through the introduction line 10H, which can cause a decrease in benzene purity in the tank.
  • a seal pot 10P is installed in the introduction part of the introduction line 10H, and the content liquid (here pure benzene) of the gas source connected via the introduction line 10H is stored in this. Then, the end of the introduction line 10H is immersed in the liquid phase in the seal pot 10P.
  • the plurality of gas sources are not limited to the same type, but may be different types such as gasoline and benzene as long as the collection targets overlap.
  • specific experimental examples performed based on each of the above-described embodiments will be described.
  • the flow rate of air containing high-concentration hydrocarbon vapor to be treated (hereinafter referred to as “source gas”) was 10 m3, and the concentration of hydrocarbon vapor was 20 vol%.
  • the components of the hydrocarbon vapor in this air were as shown in Table 1 below. (table 1 ) First, the raw material gas and the separation gas from the outlet of the vacuum pump 20 are combined, cooled in the first tube-type heat exchanger 11 and partially condensed, and then condensed into the vertical gas-liquid separator 13. And separated into gaseous and liquid phases.
  • the temperature of the gas after being cooled in the first heat exchanger 11 was 10 ° C.
  • the amount of the collected liquid hydrocarbon was 3.9 kg / hr.
  • the gas discharged from the gas-liquid separator 13 was introduced into a second tubular heat exchanger 14, where the temperature was increased.
  • the temperature of the gas after heating in this heat exchanger 14 was 30 ° C.
  • the heated gas was supplied to one of the two adsorption towers 15 where the hydrocarbon vapor was adsorbed and removed by an adsorbent.
  • the adsorbent used was a silica gel [Sili Gel CARiACT Q-3 (trade name) manufactured by Fuji Silicia Chemical Co., Ltd.] that had been subjected to hydrophobic treatment by baking at 500 ° C for 4 hours.
  • the two adsorption towers 15, 16 switched the inlet and outlet valves 23, 24, 27, 28 every 5 minutes to alternately perform adsorption and separation.
  • the concentration of hydrocarbon vapor in the gas of the adsorption tower 15, 16 exit c also was 30ppm, the components of the hydrocarbon base one par are as shown in Table 2 below.
  • the separation gas from the outlet of the vacuum pump 20 was combined with the raw material gas in the introduction line 10 and collected by cooling and condensing in the first heat exchanger 11.
  • the temperature of the adsorbent during adsorption / separation was measured with a thermocouple inserted into the adsorption towers 15 and 16, and the maximum was 35 ° C during adsorption and minimum 25 ° C during separation.
  • the air containing high-concentration hydrocarbon vapor to be treated is the same as in Experimental Example 1.
  • the raw material gas and the separation gas from the outlet of the vacuum pump 20 were combined and introduced into the vertical recovery tower 36.
  • the liquid in the liquid reservoir 19 of the recovery tower 36 is withdrawn by the pump 42, cooled in the first tubular heat exchanger 11, and then introduced into the upper part of the recovery tower 36, where it is brought into contact with the raw material gas and The hydrocarbon vapor inside was condensed.
  • the temperature of the gas after cooling in the heat exchanger 11 was 10 ° C.
  • the gas phase and the liquid phase after the gas-liquid contact were separated, and the gas phase was withdrawn from the upper part of the recovery tower 36, and the liquid phase was recovered in the lower liquid storage part 38.
  • the amount of liquid hydrocarbon collected was 3.9 kg / hr.
  • the gas discharged from the recovery tower 36 is introduced into the second plate-type heat exchanger 14. Then, the temperature was increased by heating. The temperature of the gas after heating in the heat exchanger 14 was 25 ° C.
  • the heated gas was supplied to one of the two adsorption towers 15, where the hydrocarbon vapor was adsorbed and removed by an adsorbent.
  • the adsorbent used was silica gel [Silica gel CARiACT (3-6 (trade name), manufactured by Fuji Silysia Chemical Ltd.)], which was subjected to a hydrophobizing treatment by baking at 500 ° C for 4 hours.
  • inlet and outlet valves 23, 24, 27, and 28 were switched every 5 minutes to alternately perform adsorption and separation.
  • the concentration of the hydrocarbon vapor in the gas at the outlets of the adsorption towers 15 and 16 was 30 ppm ( The components of the hydrocarbon vapor were as shown in Table 3 below.
  • the separation gas from the outlet of the vacuum pump 20 was combined with the raw material gas on the introduction line 10 and was cooled and condensed in the recovery tower 36 and recovered.
  • the temperature of the adsorbent during adsorption / separation was measured with a thermocouple inserted into the adsorption towers 15 and 16, and was found to be a maximum of 30 ° C during adsorption and a minimum of 20 ° C during separation.
  • the apparatus according to the present comparative example has a configuration in which the second heat exchanger 14 is removed from the apparatus according to the second embodiment, and the adsorption towers 15 and 16 have heating coils 45 through which steam flows.
  • Machine 46 is provided.
  • the air containing high-concentration hydrocarbon vapor to be treated is the same as in Example 1.
  • the raw material gas and the separation gas from the outlet of the vacuum pump 20 were combined and introduced into the vertical recovery tower 36.
  • the liquid in the liquid storage section 38 of the recovery tower 36 is withdrawn by the pump 42, cooled in the first tube-shaped heat exchanger 11, introduced into the upper part of the recovery tower 36, and brought into contact with the raw material gas.
  • the hydrocarbon vapor inside was condensed.
  • the temperature of the gas after cooling in the heat exchanger 11 was 10 ° C.
  • the gas phase and the liquid phase after the gas-liquid contact were separated, and the gas phase was withdrawn from the upper part of the recovery tower 36, and the liquid phase was recovered in the lower liquid storage part 38.
  • the amount of liquid hydrocarbon collected was 3.9 kg / hr.
  • the gas discharged from the recovery tower 36 was directly supplied to one of the two adsorption towers 15, where the hydrocarbon vapor was adsorbed and removed by the adsorbent.
  • the adsorbent used was silica gel [silica gel CA RiACT Q-6 (trade name) manufactured by Fuji Silica Chemical Co., Ltd.], which was subjected to hydrophobizing treatment by baking at 500 ° C for 4 hours.
  • adsorption and separation were alternately performed by switching the inlet and outlet valves 23, 24, 27 and 28 every 5 minutes.
  • the concentration of hydrocarbon vapor in the gas from the adsorption towers 15 and 16 was 100 to 200111, and a tendency to increase gradually was observed.
  • the components of the hydrocarbon vapor for the first week were as shown in Table 4 below. (Table 4)
  • the operation of separating hydrocarbons from the adsorbent in the adsorption towers 15 and 16 was performed by reducing the pressure in the adsorption towers 15 and 16 with the vacuum pump 20. The separation pressure at this time is 20 Torr in absolute pressure. This separation was performed while backflowing clean air from the outlets of the adsorption towers 15 and 16 at a flow rate of 0.5 m3 / hr.
  • the separation gas from the outlet of the vacuum pump 20 was combined with the raw material gas at the entrance of the apparatus, and was cooled and condensed in the recovery tower 36 and recovered.
  • thermocouple When the temperature of the adsorbent during adsorption and separation was measured with a thermocouple, the maximum was 15 ° C during adsorption, the minimum at 10 ° C during separation, and the maximum at 40 ° C, and rose in the adsorption towers 15 and 16. There were many times.
  • the pressure loss of the adsorption towers 15 and 16 tended to increase gradually at 20 to 30 mmH20.
  • It can be used to prevent diffusion and recovery and reuse of hydrocarbon vapor discharged from storage tanks, etc. in storage facilities for liquid hydrocarbons such as gasoline or processing facilities for refining.

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  • Separation Of Gases By Adsorption (AREA)

Abstract

L'invention se rapporte à un procédé de récupération de vapeurs d'hydrocarbures consistant premièrement à refroidir un gaz contenant une vapeur d'hydrocarbure au moyen d'un premier échangeur thermique (11) permettant de condenser ladite vapeur et à extraire une partie de la vapeur d'hydrocarbure, deuxièmement à chauffer le gaz dont une partie de la vapeur d'hydrocarbure a été extraite, au moyen d'un second échangeur thermique (14) permettant d'élever sa température, et troisièmement à transporter le gaz à température accrue jusqu'à des tours d'adsorption (15, 16) remplies d'un agent absorbant, la vapeur d'hydrocarbure étant adsorbée en vue de son extraction. On sépare l'hydrocarbure de l'adsorbant en réduisant les pressions dans les tours d'adsorption (15, 16) tout en produisant un écoulement à contre-courant de gaz propre dans les tours d'adsorption (15, 16).
PCT/JP1999/005899 1998-10-29 1999-10-26 Procede et dispositif de recuperation de vapeurs d'hydrocarbures WO2000025900A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP2000579332A JP3711327B6 (ja) 1998-10-29 1999-10-26 炭化水素ベーパーの回収方法及び装置
KR1020017005281A KR20010085967A (ko) 1998-10-29 1999-10-26 탄화수소 증기의 회수방법 및 회수장치

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JP10/308585 1998-10-29
JP30858598 1998-10-29

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WO2000025900A1 true WO2000025900A1 (fr) 2000-05-11

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003047823A (ja) * 2001-08-03 2003-02-18 Teijin Ltd 溶剤含有ガスからの溶剤除去方法
US6834686B2 (en) 2002-09-09 2004-12-28 Delaware Capital Formation, Inc. Tank pressure management system
JP2008093571A (ja) * 2006-10-12 2008-04-24 Mitsubishi Electric Corp ガス状炭化水素の処理・回収装置及びその方法
JP2009240948A (ja) * 2008-03-31 2009-10-22 Morikawa Co Ltd 溶剤の回収方法および回収装置
JP2010069435A (ja) * 2008-09-19 2010-04-02 Taikisha Ltd 溶剤回収設備
JP2011036861A (ja) * 2004-12-22 2011-02-24 Mitsubishi Electric Corp ガス状炭化水素の処理・回収装置及び方法

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP4772848B2 (ja) * 2008-10-20 2011-09-14 株式会社タツノ・メカトロニクス ベーパ回収装置

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5341345U (fr) * 1976-09-16 1978-04-10
JPS5341347U (fr) * 1976-09-16 1978-04-10
JPH10156127A (ja) * 1996-11-29 1998-06-16 I H I Plantec:Kk ベンゼンベーパー回収装置
JPH1171584A (ja) * 1997-06-17 1999-03-16 Syst Enji Service Kk ガス状炭化水素を含む廃棄ガスから炭化水素を液状で回収する方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5341345U (fr) * 1976-09-16 1978-04-10
JPS5341347U (fr) * 1976-09-16 1978-04-10
JPH10156127A (ja) * 1996-11-29 1998-06-16 I H I Plantec:Kk ベンゼンベーパー回収装置
JPH1171584A (ja) * 1997-06-17 1999-03-16 Syst Enji Service Kk ガス状炭化水素を含む廃棄ガスから炭化水素を液状で回収する方法

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003047823A (ja) * 2001-08-03 2003-02-18 Teijin Ltd 溶剤含有ガスからの溶剤除去方法
US6834686B2 (en) 2002-09-09 2004-12-28 Delaware Capital Formation, Inc. Tank pressure management system
JP2011036861A (ja) * 2004-12-22 2011-02-24 Mitsubishi Electric Corp ガス状炭化水素の処理・回収装置及び方法
JP2011072996A (ja) * 2004-12-22 2011-04-14 Mitsubishi Electric Corp ガス状炭化水素の処理・回収装置及び方法
JP2011078973A (ja) * 2004-12-22 2011-04-21 Mitsubishi Electric Corp ガス状炭化水素の処理・回収装置及び方法
JP2008093571A (ja) * 2006-10-12 2008-04-24 Mitsubishi Electric Corp ガス状炭化水素の処理・回収装置及びその方法
JP4671940B2 (ja) * 2006-10-12 2011-04-20 三菱電機株式会社 ガス状炭化水素の処理・回収装置及びその方法
JP2009240948A (ja) * 2008-03-31 2009-10-22 Morikawa Co Ltd 溶剤の回収方法および回収装置
JP2010069435A (ja) * 2008-09-19 2010-04-02 Taikisha Ltd 溶剤回収設備

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TW565468B (en) 2003-12-11
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