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WO1996036419A1 - Adsorbant preconditionne et son procede de preconditionnement - Google Patents

Adsorbant preconditionne et son procede de preconditionnement Download PDF

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Publication number
WO1996036419A1
WO1996036419A1 PCT/US1996/004516 US9604516W WO9636419A1 WO 1996036419 A1 WO1996036419 A1 WO 1996036419A1 US 9604516 W US9604516 W US 9604516W WO 9636419 A1 WO9636419 A1 WO 9636419A1
Authority
WO
WIPO (PCT)
Prior art keywords
adsorbent
vapor
vapor recovery
preconditioned
recovery system
Prior art date
Application number
PCT/US1996/004516
Other languages
English (en)
Inventor
John F. Jordan, Sr.
Original Assignee
Jordan Holding Company
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from US08/440,806 external-priority patent/US5540757A/en
Application filed by Jordan Holding Company filed Critical Jordan Holding Company
Priority to AU54402/96A priority Critical patent/AU5440296A/en
Publication of WO1996036419A1 publication Critical patent/WO1996036419A1/fr

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B67—OPENING, CLOSING OR CLEANING BOTTLES, JARS OR SIMILAR CONTAINERS; LIQUID HANDLING
    • B67D—DISPENSING, DELIVERING OR TRANSFERRING LIQUIDS, NOT OTHERWISE PROVIDED FOR
    • B67D7/00—Apparatus or devices for transferring liquids from bulk storage containers or reservoirs into vehicles or into portable containers, e.g. for retail sale purposes
    • B67D7/04—Apparatus or devices for transferring liquids from bulk storage containers or reservoirs into vehicles or into portable containers, e.g. for retail sale purposes for transferring fuels, lubricants or mixed fuels and lubricants
    • B67D7/0476—Vapour recovery 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
    • B01D53/02—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
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • 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
    • B01D2259/00—Type of treatment
    • B01D2259/40—Further details for adsorption processes and devices
    • B01D2259/401—Further details for adsorption processes and devices using a single bed
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2259/00—Type of treatment
    • B01D2259/45—Gas separation or purification devices adapted for specific applications
    • B01D2259/4516—Gas separation or purification devices adapted for specific applications for fuel vapour recovery systems

Definitions

  • the present invention relates generally to the art of recovering volatile liquids from air-volatile liquid vapor mixtures and, more particularly, to an adsorbent that has been preconditioned for vapor recovery prior to charging a reaction vessel of a vapor recovery system with the adsorbent.
  • cryogenic refrigeration systems began gaining market acceptance (note, for example, U.S. patent 3,266,262 to Moragne) . While reliable, cryogenic systems suffer from a number of shortcomings including high horsepower requirements. Further, such systems require relatively- rigorous and expensive maintenance to function properly. Mechanical refrigeration systems also have practical limits with respect to the amount of cold that may be delivered, accordingly, the efficiency and capacity of such systems is limited. In contrast, liquid nitrogen cooling systems provide more cooling than is required and are prohibitively expensive to operate for this type of application.
  • the adsorbent increases significantly in temperature. This is due to the release of the heat of adsorption of hydrocarbon and also side exothermic reactions with impurities contained in the air-hydrocarbon vapor mixture being processed. As a result of these factors, undesired and potentially unsafe overheating may occur under certain operating conditions. In order to better prevent such overheating of the beds of adsorbent, it is well known to establish a residual heel of hydrocarbons in the adsorbent prior to conducting vapor recovery processing.
  • this "preconditioning" of the adsorbent has been completed "on-site" in the actual vapor recovery system. Specifically, new/clean adsorbent is charged into the reaction vessel. The reaction vessel is then sealed and a vacuum is established. Nitrogen is then delivered to the reaction vessel to provide an inert atmosphere and gasoline vapor and nitrogen are then circulated through the reaction vessel and, therefore, the adsorbent in the bed of the reaction vessel for an extended period of time. During this gasoline vapor - nitrogen circulation, the adsorbent heats up due to the release of the heat of adsorption. Once the desired heel is established, however, the adsorbent normally cools down to near ambient temperature. After the establishment of the residual heel is verified, the vapor recovery system is ready to be returned to normal field operation.
  • the preconditioning process As this preconditioning process is performed the vapor recovery system is out of service. Accordingly, the system is unable to provide any emission control and, therefore, the terminal loading operation is also out of service. Due to the difficulty and uncertainty of preconditioning adsorbent, the preconditioning process generally takes at least 30 hours to complete and may even take up to one hundred hours in extreme conditions. As large loading terminal operations may generate revenue of up to $3 million per 24 hour period, it should be appreciated that any shut down for the preconditioning of the adsorbent leads to a substantial loss of revenue. Further, the rerouting or rescheduling of terminal loading activity through other terminal locations is troublesome, time consuming and costly. A need, therefore, is clearly identified for an improved method for changing the adsorbent in the reaction vessel beds of a vapor recovery system that significantly reduces the downtime of the vapor recovery system and, therefore, the downtime of the loading terminal.
  • a preconditioned adsorbent significantly reduces vapor recovery system downtime while also allowing one to better predict total downtime for purposes of precise scheduling and routing.
  • the method includes the steps of (1) treating the adsorbent to establish in the adsorbent a residual heel of vapor of the type to be adsorbed in subsequent vapor recovery processing and (2) adding the treated and, therefore, preconditioned adsorbent to the reaction vessel of the vapor recovery system.
  • the vapor recovery system no longer is required to be shut down for 30 to 100 hours to condition the adsorbent.
  • this leads directly to substantial revenue gains for the terminal operator.
  • the treating step includes the filling of an adsorber vessel with adsorbent, and then the sealing of the adsorber vessel.
  • Next is the evacuating of the adsorber vessel to, for example, 27 inches of mercury vacuum.
  • This is followed by the adding of nitrogen to the adsorber vessel and the circulating of a gasoline vapor and nitrogen mixture through the adsorber vessel and the adsorbent until a residual heel of vapor is established in the adsorbent.
  • the fully preconditioned adsorbent is then removed from the adsorber vessel. It is stored in air tight and water tight vessels such as DOT drums in order to prevent contamination and loss of "conditioning".
  • the preconditioned adsorbent is then simply added to the reaction vessel of the vapor recovery system which is then immediately ready for operation and terminal loading.
  • Figure 1 is a side elevational schematic representation of a processing apparatus for the preconditioning of an adsorbent in accordance with the method of the present invention.
  • FIG. 1 showing one form of apparatus 10 that may be utilized to complete the method for preconditioning adsorbent such as activated carbons or charcoal prior to the charging of a reaction vessel of a vapor recovery system with the adsorbent.
  • adsorbent such as activated carbons or charcoal
  • the apparatus 10 includes an adsorber vessel 12
  • the method includes the initial step of treating the adsorbent to establish in the adsorbent a residual heel of vapor of a type to be adsorbed in subsequent vapor recovery processing.
  • activated carbon adsorbent is being treated with hydrocarbon vapor. It should be appreciated, however, that this adsorbent and vapor are selected for purposes of illustration only and this invention is not to be considered as limited thereto.
  • This treating is completed by first filling the adsorber treatment vessel 12 with the activated carbon. More specifically, the hatch 30 is opened and the adsorber vessel 12 is filled, for example, to the seam line 32 formed between the side wall 34 and head 36 (e.g. filled with approximately 11,000 lbs of activated carbon) . The activated carbon is spread away from the fill hatch 30 and leveled as much as possible. The hatch 30 is then repositioned over the fill opening. As this is done, all activated carbon is removed from the flange around of the fill opening to insure that a good air tight seal is established. At this point, the activated carbon has not been exposed to hydrocarbon vapor levels in any appreciable amounts.
  • the initial saturation with hydrocarbon vapors is accomplished by utilizing recycled hydrocarbon vapors from the packed column absorber 18 in a nitrogen atmosphere.
  • the inert nitrogen atmosphere is necessary to reduce the risk of overheating the bed of activated carbon and thereby minimize the hazards associated therewith. More specifically, during initial saturation heat is released rapidly during the adsorption of hydrocarbons on the new activated carbon.
  • the temperature of the activated carbon in the adsorber vessel 12 is monitored closely during processing. The temperature rise occurs as a "wave front" as the hydrocarbon vapor adsorption zone works its way up through the bed of activated carbon. Temperatures as high as 200°F are commonly observed along this wave front.
  • the step of evacuating the adsorber vessel is the step of evacuating the adsorber vessel. More specifically, the sparger valves 38, 40 and 42 and vacuum control valve 44 are all opened. The port of valve 44 is then connected to a vacuum pump 48. With the flow control valves 20, 22, 24 and 26 as well as adsorber vessel drain valve 50 all closed vacuum pump 48 is operated to establish a vacuum of, for example, 27 inches of mercury vacuum in the absorber vessel 12. Once established, the vacuum control valve 44 is closed. The vacuum in the adsorber vessel 12 is then monitored for a short period of time to insure that there are no air leaks. If a leak is discovered, the leak is identified and a proper seal is established.
  • the steps just described are then repeated to establish the 27 inches of mercury vacuum in the adsorber vessel 12.
  • the port of control valve 44 is now connected to a source of nitrogen 52.
  • a regulator on the nitrogen source 52 is set for 100-125 psig and the control valve 44 is opened. This allows nitrogen to begin to bleed into the adsorber vessel 12.
  • the delivery of nitrogen to the adsorber vessel 12 continues through the control valve 44 until the vacuum gage 54 reads 0 vacuum (e.g. until approximately 650 ft 3 of nitrogen are delivered) .
  • the port of control valve 44 is then reconnected to the vacuum pump 48 and a vacuum is again drawn down to 27 inches of mercury vacuum in the adsorber vessel 12.
  • Nitrogen is then reintroduced into the adsorber vessel 12 for a second time in the manner previously described until the vacuum gage 54 reads 0 vacuum. A 27 inches of mercury vacuum is then reestablished in the adsorber vessel 12 for a third time in the. manner previously described. Nitrogen is then introduced into the adsorber vessel 12 for a third time also in the manner previously described until the vacuum gage 54 again reads 0 vacuum. At this time the control valve 44 is closed and this portion of the procedure for establishing an inert atmosphere in the adsorber vessel 12 is completed.
  • blower 56 and packed column absorber 18 are purged by nitrogen to displace as much air as possible, specifically, the nitrogen source 52 is connected to the port of valve 58 and valves 58 and 60 are opened so that nitrogen flows through the blower 56 and the packed column absorber 18. Once purging is completed, the valves 58 and 60 are closed.
  • the packed column absorber 18 is filled with fresh gasoline to a predetermined level (e.g. with approximately 100 gallons) .
  • a source of gasoline 62 is connected to the port of valve 64: valve 64 being opened to allow the delivery of gasoline to the packed column absorber 18.
  • the valve 64 is closed.
  • valves 22 and 26 are opened and blower 56 and gasoline pump 66 are activated and gasoline is sprayed into the packed column absorber 18 by means of the sprayer 67.
  • gasoline vapors are circulated in a predominately inert nitrogen atmosphere from the packed column absorber 18 to the adsorber vessel 12 (and the activated carbon contained therein) and back again in a closed loop through the conduits 14, 16.
  • This circulating step is continued for, approximately, 15 to 50 hours.
  • a particular level e.g. 8 RVP
  • the hatch 30 of the adsorber vessel 12 is carefully opened to allow venting to atmosphere and a sample of preconditioned carbon is carefully removed from the adsorber vessel. This sample is weighted to insure that a proper gasoline heel has been established. If not, the nitrogen atmosphere is reestablished and the saturation loop just described (wherein gasoline vapor flows between the packed column absorber 18 and the adsorber vessel 12) is reinitiated until the proper heel weight has been established.
  • the next step in quality control is to purge the entire system with air and restart the saturation loop. If the carbon vessel temperatures remain steady, the saturation process is complete. If the temperatures do not remain below 100°F, the saturation loop is continued until all temperatures are again below 100°F.
  • valves 20, 22, 24 and 26 are closed and pump 66 and blower 56 are again deactivated.
  • the carbon vessel fill hatch 30 is then opened.
  • the valve 60 may be open to atmosphere to alleviate any system pressure.
  • valve 50 is opened to drain the preconditioned activated carbon from the vessel 12.
  • the preconditioned carbon may be collected in an air tight and water tight drum for shipping to the end user if desired.
  • Following shipping, is the adding of the treated and preconditioned activated carbon to the reaction vessel of the vapor recovery system of the customer.
  • the vapor recovery system is made substantially immediately ready for vapor recovery processing.
  • the prior art approach of "on-site" conditioning of the activated carbon in the vapor recovery system can lead to further significant complications.
  • the activated carbon may not cool down properly so that gasoline loading may resume.
  • the activated carbon cannot effectively adsorb hydrocarbons for up to six weeks. Therefore, the associated loading terminal is only able to operate out of EPA compliance and may possibly need to be shut down for the entire period.
  • the present method for preconditioning an adsorbent off site in a controlled situation serves to significantly reduce the cost, downtime, and uncertainty associated with the prior art method of conditioning the carbon "on-site" after it is charged into the reaction vessel of the vapor recovery system.
  • the end user is effectively provided with a large economic benefit as vapor recovery system downtime is reduced by up to 30-100 hours. Accordingly, 30 to 100 hours of revenue generation are restored to the terminal operator.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

L'invention décrit un procédé de préconditionnement d'un adsorbant, tel qu'un charbon actif, avant d'ajouter l'adsorbant dans le réacteur d'un système de récupération de vapeur. Le procédé comprend les étapes suivantes: (1) traitement de l'adsorbant pour créer un résidu de fond de réservoir du type que l'on peut adsorber ultérieurement lors du processus de récupération de vapeur et (2) ajout de l'adsorbant traité, et donc préconditionné, au réacteur du système de récupération de vapeur. Cette invention permet de réduire de façon significative le temps d'immobilisation du système de récupération de vapeur.
PCT/US1996/004516 1995-05-15 1996-04-02 Adsorbant preconditionne et son procede de preconditionnement WO1996036419A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU54402/96A AU5440296A (en) 1995-05-15 1996-04-02 Method for preconditioning adsorbent and preconditioned adso rbent

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US08/440,806 US5540757A (en) 1995-05-15 1995-05-15 Method for preconditioning adsorbent
US08/440,806 1995-05-15
US58762696A 1996-01-17 1996-01-17
US08/587,626 1996-01-17

Publications (1)

Publication Number Publication Date
WO1996036419A1 true WO1996036419A1 (fr) 1996-11-21

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ID=27032563

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US1996/004516 WO1996036419A1 (fr) 1995-05-15 1996-04-02 Adsorbant preconditionne et son procede de preconditionnement

Country Status (3)

Country Link
AU (1) AU5440296A (fr)
CA (1) CA2193687A1 (fr)
WO (1) WO1996036419A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7629463B2 (en) 2001-08-15 2009-12-08 E. I. Du Pont De Nemours And Company Ortho-heterocyclic substituted aryl amides for controlling invertebrate pests

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1088029B (de) * 1955-03-30 1960-09-01 Lab Fuer Adsorptionstechnik G Verfahren zur Abtrennung und Gewinnung von wasserloeslichen Loesemitteln aus Gasen durch Adsorption
FR1351661A (fr) * 1963-02-06 1964-02-07 Metallgesellschaft Ag Procédé pour empêcher le chauffage excessif d'agents d'adsorption pendant la récupération de solvants facilement décomposables
US4128405A (en) * 1977-02-16 1978-12-05 Continental Oil Company Incomplete drying of activated carbon in a process for VCM reduction in vapors
US4830735A (en) * 1986-12-19 1989-05-16 Labofina, S.A. Process for removing carbonyl-sulfide from liquid hydrocarbon feedstocks
US5493035A (en) * 1995-03-24 1996-02-20 Arco Chemical Technology, L.P. Propylene oxide purification

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1088029B (de) * 1955-03-30 1960-09-01 Lab Fuer Adsorptionstechnik G Verfahren zur Abtrennung und Gewinnung von wasserloeslichen Loesemitteln aus Gasen durch Adsorption
FR1351661A (fr) * 1963-02-06 1964-02-07 Metallgesellschaft Ag Procédé pour empêcher le chauffage excessif d'agents d'adsorption pendant la récupération de solvants facilement décomposables
US4128405A (en) * 1977-02-16 1978-12-05 Continental Oil Company Incomplete drying of activated carbon in a process for VCM reduction in vapors
US4830735A (en) * 1986-12-19 1989-05-16 Labofina, S.A. Process for removing carbonyl-sulfide from liquid hydrocarbon feedstocks
US5493035A (en) * 1995-03-24 1996-02-20 Arco Chemical Technology, L.P. Propylene oxide purification

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7629463B2 (en) 2001-08-15 2009-12-08 E. I. Du Pont De Nemours And Company Ortho-heterocyclic substituted aryl amides for controlling invertebrate pests

Also Published As

Publication number Publication date
AU5440296A (en) 1996-11-29
CA2193687A1 (fr) 1996-11-21

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