WO1993016808A1 - Method of and apparatus for making inerted closed spaces - Google Patents

Method of and apparatus for making inerted closed spaces Download PDF

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Publication number
WO1993016808A1
WO1993016808A1 PCT/HU1992/000010 HU9200010W WO9316808A1 WO 1993016808 A1 WO1993016808 A1 WO 1993016808A1 HU 9200010 W HU9200010 W HU 9200010W WO 9316808 A1 WO9316808 A1 WO 9316808A1
Authority
WO
WIPO (PCT)
Prior art keywords
inert gas
closed space
oxygen
air
closed
Prior art date
Application number
PCT/HU1992/000010
Other languages
French (fr)
Inventor
Endre GULYÁS
Árpád KOLLÁR
Ferenc Mózer
Original Assignee
Richter Gedeon Vegyészeti Gyár Rt.
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
Application filed by Richter Gedeon Vegyészeti Gyár Rt. filed Critical Richter Gedeon Vegyészeti Gyár Rt.
Priority to PCT/HU1992/000010 priority Critical patent/WO1993016808A1/en
Publication of WO1993016808A1 publication Critical patent/WO1993016808A1/en

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/14Production of inert gas mixtures; Use of inert gases in general
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B04CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04BCENTRIFUGES
    • B04B15/00Other accessories for centrifuges
    • B04B15/08Other accessories for centrifuges for ventilating or producing a vacuum in the centrifuge
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B04CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04BCENTRIFUGES
    • B04B7/00Elements of centrifuges
    • B04B7/02Casings; Lids
    • B04B7/06Safety devices ; Regulating

Definitions

  • the present invention makes it possible to save a substantial quantity of inert gas since positive flushing itself takes place only when the working space is gas tightly closed. Another advantage is in it that the inert gas atmosphere within the working space remains unchanged even in emergency cases. An important advantage is to be seen in it that the working space can be opened only when there is no emergency situation and said space is already containing air rather than inert gas. A further advantage is in it that the inert gas supply system suffers no shocklike loading.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Centrifugal Separators (AREA)

Abstract

The present invention relates to methods of and apparatuses for making inerted closed spaces, especially the interior of containers being parts of chemical equipments. Inert gas under overpressure will be supplied into the closed space and at least a part of the oxygen of the air will be pushed out therefrom by means of said inert gas. By means of continuous inert gas replacement, oxygen concentration will be kept under a predetermined level. After ending of the prescribed working procedure said overpressure will be ceased and said closed space will be opened. Gas tightness of the closed space will be checked prior to begin with pushing out the oxygen of the air, said checking being made by observing the pressure of the closed space during letting in inert gas at reduced rate. Pushing out the oxygen of the air at full rate of inert gas supply will be started only after a prescribed pressure value being observed during letting in said inert gas at said reduced rate.

Description

METHOD OF AND APPARATUS F.OR MAKING INERTED CLOSED SPACES
Technical field
The present invention relates to methods of and apparatuses for making inerted closed spaces, especially the interior of containers being parts of chemical equipments.
Background of the invention
During operation of certain chemical equipments (for example industrial centrifuges) the material to be treated often contains inflammable and/or explosive components (for example solvents) which in the presence of the oxygen of the air may inflame and cause fire and/or explosion. Therefore, closed spaces (vessels, container.s) of such equipments have to be made free of oxygen by means of filling them with an inert gas.
In GB-PS 2 010 706, there is described a solution of making inert the interior of centrifuges. The spirit of that solution is in it that prior to begin the centrifuging the closed working space is flushed by an inert gas (for example nitrogen) displacing therefrom both oxygen and inflammable gases and vapours being present. It is secured by means of different interlocking and controlling means that the centrifuge can be started only when inlet of a predetermined volume of the inert gas is finished. When the closed space becomes opened the flushing procedure will be restarted. The inlet velocity of the inert gas is controlled and with inappropriate velocity values an emergency signal is given out. -
During the centrifuging procedure slight overpressure is maintained within the closed space in. order to prevent entering of ambient air. With diminishing overpressure an emergency signal is given out.
In certain cases measuring of oxygen content of the flushing gas leaving the closed space is recommended in order to obtain an emergency signal when flushing of the space is insufficient.
It is a drawback of the above solution that checking of the inert gas inlet by volumetry does not give sufficient information as to having made the closed space free enough of dangerous components. For example, when the working space is not properly closed for some reason, inlet of prescribed volume of the inert gas would not result in proper inerting since -a part of the inert gas would escape at unsealed point and oxygen concentration could remain over the permitted valu
Another drawback is in it that in case of an emergency switch off continuous inert gas supply of the closed space is not maintained.
A further deficiency of the known solution is in it that with finished centrifuging inert gas atmosphere remains within the closed space. Therefore, personnel of the equipment can suffer grave accidents or even may be killed by the suffocating inert gas.
Still further drawback of the known solution is to be seen in it that opening of the machine casing can happen prior to complete stopping of rotation. Thus the rotating centrifuge can produce ignition sparks when air enters the working space which is already open. Object of .the present invention is to eliminate the drawbacks mentioned above.
Therefore, main goal of the present invention is to produce a method of and an apparatus for making inerted closed spaces with improved security and without wasting of the inert gas.
Summary of the invention
There is invented a method of making inerted closed spaces, especially the interior of containers being parts of chemical equipment, during which inert gas will be supplied under overpressure into said closed space, and at least a part of the oxygen of the air will be pushed out therefrom by means of said inert gas, further keeping the oxygen concentration under a predetermined level by means of continuous inert gas replacement, and after ending of a prescribed working procedure said overpressure will be ceased and said closed space will be opened according to prevailing demands, the improvement of said method being in checking the gas tightness of the closed space prior to begin with pushing out the oxygen of the air, said checking being made by observing pressure of said closed space during letting in inert gas at reduced rate, and said pushing out of the oxygen of the air at full rate of inert gas supply being started only after a prescribed pressure value bein.; observe - during letting in said inert gas at said reduced rate.
It is of advantage to maintain said inert gas supply even when said working procedure within the closed space must be stopped upon some emergency situation. It is also of advantage to create underpressure within the closed space after ending of the working procedure made within said closed space and sucking in air by means of said underpressure until there is restituted an atmosphere which is not harmful to human health.
Preferably, full stop of any motion within said closed space can be sensed as well, whereas opening of said space will be effected only thereafter.
There is also invented an apparatus for making inerted closec spaces, especially the interior of containers being parts of chemical equipments, said apparatus having inert gas line, and vent line both connected with said closed space, pressure gauge checking the pressure within said closed space and shut-off means associated with said lines, the improvement of said apparatus being in it that it has a switch connected to a control unit fitted with means for stopping supply of said inert gas.
It is of advantage when said closed space is connected with a vacuum source through a shut-off means, preferably vacuum valve, and the line supplying inert gas into' said closed space is in connection with the ambient atmosphere through a draw in valve.
Further it is of advantage when a rotation sensing means is associated with a working organ within said closed space, and said rotation sensing means is connected to said control unit. Brief description of the drawing
The invention will now be described in connection with an example referring to the accompanying drawing which shows schematic layout of the apparatus according to the example.
Detailed description of the preferred embodiment
The apparatus as shown in the drawing is associated with a centrifuge 12 of gas-tightly sealed construction. The closed inner space of the centrifuge 12 is connected to an inert gas supply 1 through first line 10, first rate-of-flov; meter 9, further control unit 5, pressure reducer 3 and first shut-off means 2. Bearing box of the centrifuge 12 is also connected to the inert gas supply 1 through second line 8, second rate-of-flow meter 7, further the control unit 5, the pressure reducer 3 and the first shut-off means 2. The control unit 5 is fitted with a pressure gauge 6 which is connected through check line 19 to the critical uppermost point of the closed inner space of the centrifuge 12.
The centrifuge 12 has a coverlock 13 fitted with a position signalling means connected with the control unit 5 and a cover turn down sensing means 14 signal output of which is also connected to the control unit 5. Finally a rotation sensing means 16 of the centrifuge 12 is similarly connected to the control unit 5. These connections are made by means of control lines 26.
First line 10 is in connection with the ambient atmosphere through a stub fitted with a draw in valve 11. The centrifuge 12 further has a liquid let off 17 fitted with an inert gas barrier 18 and a vent line 20 fitted with a pressure limiting means 22 (for example a spring-loaded back valve) representing a constant resistance against the outflowing - - 6 -
gas. The section of the vent line 20 between the pressure limiting means 22 and the centrifuge 12 is connected to a vacuum source (not shown) through vacuum valve 21. The vacuum valve 21 is operated by the control unit 5 through one of the lines 26. The centrifuge 12 further has an electric switch 24 which is also connected to the control unit 5. The lines 19, 20 are in connection with an oxygen concentration gauge 25 signal output of which is connected to the control unit 5.
Vent line 23 of the bearing box of the centrifuge 12 is connected to the vent line 20 of the working space of the centrifuge 12 between the pressure limiting means 22 and that end of the vent line 20 which is open to the ambient atmosphere. The centrifuge 12 further has a swinging sensor 15 signal output of which is also connected to the control unit 5.
The control unit 5 is preferably a pneumatic one and comprises logic elements and control structures (not shown) supplied by energy through supply line 4. Since the control unit 5 can be realised on the base of known principles by simple construction work detailed description of the structure thereof is considered as superfluous.
The method according to the invention will be realised by means of the above apparatus as follows:
The apparatus can be actuated only after the control unit 5 receives-signals—from the cover turn down sensing means 14 and the position signalling means of the coverlock 13 stating both turned down position of the cover and locked position of the coverlock, further receives signal from the rotation sensing menas 16 stating that the centrifuge 12 does not rotate. Bering box of the centrifuge 12 is continuously held under nitrogen atmosphere, whereas the working -space will be flushed by nitrogen gas for the time and at the rate as required by the prevailing technology.
Prior to start the apparatus it must be checked that in the inert gas supply line 4 there is sufficient pressure. Than all openings of the centrifuge 12 (cover, let out etc.) will be gas-tightly closed.
At starting, the inert gas will enter the centrifuge 12 through line 8 at a constant rate, whereas through line 10 at a rate reduced as compared with the rate-of-flow at normal working. Said rates are checked by rate-of-flow meters 7 and 9. If within the working space there is established the prescribed flushing pressure the control unit 5 receives a signal through check line 19. On the base thereof the control unit 5 will let flush the centrifuge 12 for the prescribed time of' flushing and at the prescribed rate (which is higher than that of the previous checking). If during the check flushing (pre-flushing) there is not established the prescribed pressure value an emergency signal is generated and normal flushing will not be started. In this case proper closing of all openings should be checked again. Source of error may be for example the partly closed cover or removal of the unloading vehicle.
After elapsing of the flushing time the control unit 5 will reduce the rate-of-flow of the inert gas in such extent that only a slight normal working overpressure remains within the~working" space. The value of this overpressure is sensed by the control unit 5 and shown by pressure gauge 6. When this value is proper the centrifuge 12 can be started, the material to be treated can be loaded in, centrifuged, washed and peeled off. After finished centrifuging the cover cannot be opened until full stop of the centrifuge i.e. until the rotation sensing means 16 does not give out the corresponding signal. Until this moment the inert gas atmosphere and the working mode overpressure remain unchanged within the working space. When the centrifuge is fully stopped the supply of the inert gas will be interrupted, the control unit 5 let the vacuum valve 21 open and the pressure limiting means 22 will automatically close. Therefore, a slight vacuum (for example 3 to 4 kPa) will be created within the working space of the centrifuge, the .draw in valve 11 will automatically open and air will flow into the working space through line 10. After a pre¬ determined venting time control unit 5 releases the lock of the cover of centrifuge 12, i.e. unloading thereof can take place.
That means that there is always an inert gas atmosphere within the centrifuge when the machine is rotating and can produce ignition sparks, and it can be opened only when thoroughly ventillated by air.
The control unit 5 is checking sure operation of rotation sensing means 16 as well. In case of its failure control unit 5 will automatically stop the centrifuge 12. Similar stopping will happen when swinging sensor 15 signalizes shaking of the centrifuge or when there is no sufficient overpressure within the centrifuge or when there is no energy supply or when the pressure of the inert gas supply is insufficient. In all these cases emergency signal(s) will be -given out by control unit 5, and the centrifuge"will be stopped but remains under inert gas atmosphere and its cover cannot be opened. After removing of the failure locking of the cover can be released, the control unit is returned to starting position and the inerting procedure (checking, flushing etc. ) can be started again. The present invention makes it possible to save a substantial quantity of inert gas since positive flushing itself takes place only when the working space is gas tightly closed. Another advantage is in it that the inert gas atmosphere within the working space remains unchanged even in emergency cases. An important advantage is to be seen in it that the working space can be opened only when there is no emergency situation and said space is already containing air rather than inert gas. A further advantage is in it that the inert gas supply system suffers no shocklike loading.
Of course, the invention can be used not only with centrifuge but also with autoclaves and other equipments.

Claims

1. A method of making inerted closed spaces, especially the interior of containers being parts of chemical equipments, during which" inert gas will be supplied under overpressure into said closed space, and at least a part of the oxygen of the air will be pushed out therefrom by means of said inert gas, further the oxygen concentration will be kept under a predetermined level by means of continous inert gas replace¬ ment, and after ending of a prescribed working procedure said overpressure will be ceased and said closed space will be opened according to prevailing demands, characterized by checking the gas tightness of the closed space prior to begin with pushing out of the oxygen of the air, said checking being made by observing pressure of the closed space during letting in inert gas at reduced rate, and said pushing out of the oxygen of the air at full rate of inert gas supply being started only after a prescribed pressure value being observed during letting in said inert gas at said reduced rate.
2. A method according to Claim 1, characterized by main¬ taining the inert gas supply even when the working procedure must be stopped within the closed space upon some emergency situation.
3.. A method according to Claim 1 or Claim 2, characterized by creating underpressure within the the closed space after ending of"the working procedure made within said closed space and sucking in air by means of said underpressure until there is restituted an atmosphere which is not harmful to human health.
4. A method according to anyone of Claims 1 to 3 , characterized by sensing full stop of any motion within said closed space and opening thereof being effected only there¬ after.
5. An apparatus for making inerted closed spaces, especially the interior of containers being parts of chemical equipments, said apparatus having inert gas line and vent line both connected with said closed space, pressure gauge checking the pressure within said closed space and shut-off means associated v.'ith said lines, characterized by having a switch (24) connected to a control unit (5) fitted with means for stopping supply of said inert gas.
6. An apparatus according to Claim 5, characterized by said closed space being connected with a vacuum source through a shut-off means, preferably vacuum valve (21), and the line (10) supplying inert gas into said closed space being in connection with the ambient atmosphere through a draw in valve (11).
7. An apparatus according to Claim 5 or Claim 6, characterized by a rotation sensing means (16) associated with a working organ arranged within said closed space, said rotation sensing means (16) being connected to said control unit ( 5 ) .
PCT/HU1992/000010 1992-02-24 1992-02-24 Method of and apparatus for making inerted closed spaces WO1993016808A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PCT/HU1992/000010 WO1993016808A1 (en) 1992-02-24 1992-02-24 Method of and apparatus for making inerted closed spaces

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/HU1992/000010 WO1993016808A1 (en) 1992-02-24 1992-02-24 Method of and apparatus for making inerted closed spaces

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0700715A3 (en) * 1994-09-12 1996-04-17 Messer Griesheim Gmbh
WO2018114046A1 (en) * 2016-12-21 2018-06-28 Apk Ag Gas-tight centrifuge for separating solids from a polymer solution, and method for separating solids from a polymer solution
DE102017123999A1 (en) * 2017-10-16 2019-04-18 Heinkel Holding Gmbh Separator for substances with a centrifuge and method for inerting the separator
CN111655380A (en) * 2017-12-20 2020-09-11 埃佩多夫股份公司 Temperature controllable centrifugal machine

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2010706A (en) * 1977-04-22 1979-07-04 Marl Associates Ltd Centrifuges
EP0335278A2 (en) * 1988-03-31 1989-10-04 E.I. Du Pont De Nemours And Company Evacuation pump control for a centrifuge instrument

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB2010706A (en) * 1977-04-22 1979-07-04 Marl Associates Ltd Centrifuges
EP0335278A2 (en) * 1988-03-31 1989-10-04 E.I. Du Pont De Nemours And Company Evacuation pump control for a centrifuge instrument

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0700715A3 (en) * 1994-09-12 1996-04-17 Messer Griesheim Gmbh
WO2018114046A1 (en) * 2016-12-21 2018-06-28 Apk Ag Gas-tight centrifuge for separating solids from a polymer solution, and method for separating solids from a polymer solution
DE102017123999A1 (en) * 2017-10-16 2019-04-18 Heinkel Holding Gmbh Separator for substances with a centrifuge and method for inerting the separator
DE102017123999B4 (en) 2017-10-16 2021-07-22 Heinkel Holding Gmbh Separating device for substances with a centrifuge and method for inerting the separating device
CN111655380A (en) * 2017-12-20 2020-09-11 埃佩多夫股份公司 Temperature controllable centrifugal machine
US20210001352A1 (en) * 2017-12-20 2021-01-07 Eppendorf Ag Temperature-controlled Centrifuge
CN111655380B (en) * 2017-12-20 2022-04-15 埃佩多夫股份公司 Temperature controllable centrifugal machine
US11577257B2 (en) * 2017-12-20 2023-02-14 Eppendorf Ag Temperature-controlled centrifuge with protective gas release in case of rotor crash

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