Europisches Patentamt

(19)

European Patent Office

*EP000701099B1*

Office europen des brevets

(11)

EP 0 701 099 B1

EUROPEAN PATENT SPECIFICATION

(12)

(45) Date of publication and mention

(51) Int Cl.7:

of the grant of the patent:

26.09.2001 Bulletin 2001/39

F25J 3/04

(21) Application number: 95402053.3

(22) Date of filing: 11.09.1995
(54) High purity nitrogen production process
Verfahren zur Herstellung von hochreinem Stickstoff
Procd de production dazote de haute puret
(84) Designated Contracting States:
DE FR GB IT NL

(30) Priority: 12.09.1994 US 312248

(43) Date of publication of application:
13.03.1996 Bulletin 1996/11

(72) Inventor: Ha, Bao

Vacaville, California 95688 (US)

(74) Representative: Vesin, Jacques et al

LAIR LIQUIDE, S.A.,
Service Proprit Industrielle,
75, Quai dOrsay
75321 Paris Cdex 07 (FR)

(73) Proprietor: AIR LIQUIDE PROCESS &

EP 0 701 099 B1

CONSTRUCTION, INC.
Houston, Texas 77056 (US)

(56) References cited:

EP-A- 0 542 405
EP-A- 0 611 936

EP-A- 0 592 323

JP-A- 3 230 079

Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give
notice to the European Patent Ofce of opposition to the European patent granted. Notice of opposition shall be led in
a written reasoned statement. It shall not be deemed to have been led until the opposition fee has been paid. (Art.
99(1) European Patent Convention).
Printed by Jouve, 75001 PARIS (FR)

EP 0 701 099 B1

Description
[0001] The present invention relates to a process for
the production of at least one nitrogen product having
an extremely low level of detectable contaminants and
impurities, or an "ultra-pure" nitrogen product.
[0002] Variations on traditionally available air separation processes to make high purity nitrogen have been
proposed to reduce levels of impurities, such as hydrogen, helium, oxygen, carbon monoxide, hydrocarbons
and neon, as concentrations of these constituents in
cooled and dried feed air may be as high as 20 ppm.
Some of these processes have been successful to reduce impurities in the nitrogen product to low levels.
[0003] The semiconductor industry in particular demands levels of contaminants and impurities in process
gases to be maintained at an extremely low level, often
required to be maintained at or below 10 ppb. Together
with the ultra-pure nitrogen requirement, often at the
same or nearby facility a gas consumer may have requirements for nitrogen gas of more normal purity, and
the relative as well as total volumes required may vary
from time to time. These and other factors require new
and improved cost-sensitive and flexible processes for
separating air into nitrogen products of varying purity,
including production of extremely ultra-pure nitrogen.
[0004] US-A-5 218 825 discloses a process for producing both a normal purity and a high purity nitrogen
product. Air is compressed, cooled and flowed to a main
column operating at or near nitrogen product pressure,
wherefrom a nitrogen-enriched stream is withdrawn and
a normal purity nitrogen product is taken prior to the nitrogen-enriched stream being increased in pressure
and returned to the main column, following expansion,
as reflux. According to the process described, a side
rectification column takes a feed from the stripping section of the main column and a high purity nitrogen product is produced in the upper portion of the side rectification column. The process utilizes expansion of the oxygen-enriched stream from the bottom of the main column to condense vapors at the top of the main air separation column.
[0005] US-A-5 123 947 discloses a multi-column cryogenic air distillation where ultra-high purity nitrogen,
defined as typically less than 0.1 ppm impurities is produced from a nitrogen-rich stream withdrawn from a first
column and fed to a second column. The process describes purging a portion of uncondensed vapor produced from the top of a second column, and recovering
the ultra-high purity nitrogen product at a point below
the purge point in the second column.
[0006] US-A-4 902 321 discloses a process for the
production of high purity nitrogen comprising partial condensation of a nitrogen rich vapor stream containing
light impurities withdrawn from a main cryogenic air distillation column by indirect heat exchanger with the expanded condensate in a heat exchanger.
[0007] In US-A-5 325 674 a process is disclosed for

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producing high purity nitrogen comprising expanding a

dried and cooled feed air stream into a first air separation column to produce a nitrogen-enriched stream at
the top of the column. Also disclosed is the flowing of
recycled nitrogen at an elevated pressure through a reboiler located in the lower portion of a second column
to provide boil-up, and thereafter flowed into the upper
portion of the second column, to produce at the top of
the second column vapors containing light impurities
which vapors after at least partially condensing in a condenser located in the lower portion of the air separation
column, are purged from the second column. High purity
nitrogen is produced from the lower portion of the second column.
[0008] EP-A-0 376 465 discloses a method of purifying nitrogen from an air separation process and producing an high purity nitrogen product by charging a nitrogen-enriched stream from a conventional air separation
process to the bottom of a column having a reflux condenser. Liquid nitrogen is withdrawn from an upper portion of the column and flashed to generate a liquid and
a vapor. The liquid from the flash separation is recovered and flashed a second time to produce the high purity product.
[0009] J-A-03230079 and EP-A-0589766 disclose a
process for separating air in which air is sent to a first
column, oxygen-enriched liquid from the bottom of the
column is sent to a top condenser, nitrogen-enriched
gas is removed from the top of the first column, compressed and sent to the bottom of a second column
whose top gas is used to reboil the first gas. Product
nitrogen is removed from the top of the first column.
EP-A-0611936 discloses a process having the
features of the preamble of Claim 1.
An improved process and installation to effectively
carry out the production of both ultra-high purity nitrogen
and a normal purity nitrogen would be advantageous
and is much desired.
[0010] Processes according to the invention are as
defined in Claim 1.
A feature of one process in accordance with the
present invention is to provide a flexible and economical
method for production of nitrogen products of differing
purity.
[0011] By the term "substantially free", it is meant a
concentration of less than about 50 parts per billion.
[0012] In other embodiments, the process according
to the present invention further comprises production of
a normal purity nitrogen product and optionally a second
nitrogen product of higher purity. The higher purity
stream is substantially free of heavy hydrocarbon contaminants, and in the preferred embodiment also substantially free of light impurities. The preferred embodiments of the present invention are particularly advantageous to the art of producing high purity nitrogen, among
other factors, due to the expansion of feed air directly
into the air separation column, and therefore the ability
to operate the separation columns at relatively low pres-

EP 0 701 099 B1

sure.
[0013] Figure 1 represents schematically an installation for producing high purity nitrogen products substantially free of heavy contaminants and light impurities.
[0014] Figure 2 represents schematically further embodiments of the present invention to enable production
of high purity nitrogen products.
[0015] Figure 1 schematically depicts various process
components and process options which comprise various embodiments of the present invention. The processes and installations depicted in Figure 1 provide for
the production of extremely pure nitrogen in an integrated cryogenic environment. In the preferred embodiment, the process comprises taking a compressed and
dried feed stream 101, which comprises major amounts
of nitrogen and oxygen, and minor amounts of impurities
and contaminants, and cooling at least a portion of the
feed air in heat exchanger 40 in a heat exchange relationship with one or more other process streams. When
exiting the heat exchanger 40, the cooled feed stream
103 is expanded in a turbine 80 to form expanded feed
stream 105 which is thereafter flowed into air separation
column 10 at an intermediate point in the column between stripping zone 19 and rectifying zone 14. Preferably the column 10 is maintained between about 3 bar
and about 4.5 bar absolute. The expansion of cooled
feed stream 103 provides cold for liquefaction and separation of the feed air in the air separation column 10 to
form at the bottom of the column an oxygen enriched
liquid, and at the top of the column a nitrogen-enriched
vapor. The stripping zone 19 and rectifying zone 14 may
comprise any of well-known vapor-liquid contacting
means, such as sieve trays, bubble cap trays, and structured or random-type packings.
[0016] Nitrogen-enriched vapor stream 201 is withdrawn from the upper portion of the column 10 and
warmed against at least one other process stream in
subcooler 20 and main heat exchanger 40. At least a
portion of the withdrawn and warmed stream 205 is
compressed in recycle compressor 60 to a pressure
greater than the column 10 pressure, preferably to between about 4 bar and about 10 bar. In accordance with
the process of the present invention, at least a portion
of the compressed nitrogen-enriched stream is cooled
in main exchanger 40 flowed to a second column, which
operates at a pressure greater than the pressure of the
air separation column 10, which operates preferably between about 4 bar and about 10 bar absolute. The intermediate nitrogen stream 211 enters the second column 30 at a point below a vapor liquid contacting zone
37. Nitrogen vapors rise in contacting zone 37, and at
least a portion of the rising nitrogen vapors are condensed against cooler oxygen-enriched liquid contained
in the bottom of air separation column 10 in condenser
70. Condensed nitrogen vapors are returned to the upper portion of the second column 30, and descend
downward through contacting section 37 whereby
heavy contaminants which may comprise carbon mon-

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oxide, argon, residual oxygen, and heavier hydrocarbons are absorbed from the nitrogen vapors into the descending liquid and are concentrated in the bottom of
the second column 30. A portion 307 of the liquid nitrogen concentrated in heavy contaminants is removed
form the bottom of the second column 30, and preferably
cooled and expanded, and thereafter flowed to the air
separation column 10, where it is preferably fed to column 10 at an intermediate location. By the term "heavy
contaminants", it is meant constituents which are less
volatile than nitrogen, and by the term "light impurities"
it is meant those constituents which are more volatile
than nitrogen. Typical heavy contamiants include oxygen, carbon monoxide, argon, hydrocarbon compounds, krypton, xenon, carbon dioxide and water. Typical light impurities include hydrogen, helium and neon.
[0017] In accordance with the embodiments of Figure
1, a nitrogen-enriched stream substantially free of heavy
contaminants is withdrawn from the upper portion of the
second column in conduit 301 and flowed (via 505)to a
third column 50, which is preferably operated at a pressure between that of the column 10 and the second column 30, preferably between about 3.5 bar and 9 bar absolute, wherein light impurities are distilled from the nitrogen stream 301 in a stripping zone. Preferably, the
nitrogen feed stream 301 is flowed through a reboiler 90
located in the lower portion of column 50 to provide boilup for the column, and thereafter at least a portion of the
feed stream exiting from condenser 90 is expanded into
column 50 at a point above a vapor-liquid contacting
zone, wherein light impurities remain in rising vapors
and are concentrated in a vapor stream 59 removed
from column 50 and optionally expanded into an upper
location in air separation column 10. A vapor stream
above reboiler 90, and a liquid accumulation below reboiler 90 in column 50, substantially free of both heavy
contaminants and light impurities, is thus available, as
ultra-pure gaseous nitrogen in conduit 56, and optionally
liquid nitrogen in stream 55. Gaseous ultra-pure nitrogen withdrawn in conduit 56 is warmed in heat exchanger 40 and made available to the gas user requiring extremely high purity nitrogen product.
[0018] Referring now again to the air separation column 10 of Figure 1, in preferred embodiments oxygenenriched liquid is withdrawn via line 131 from below the
contacting zone 19, cooled against other process
streams in subcooler 20 from which it flows via line 132,
and expanded into tho top condenser area of column 10
where it vaporizes to condense in heat exchanger 110
at least a portion of the nitrogen-enriched vapors rising
in the upper portion of the column. Following condensation in condenser 110, nitrogen condensation is returned
to the column as reflux, and vaporized oxygen-enriched
stream 135 exits the top condenser area and after being
warmed against other steams in heat exchangers 20
and 40, flows from the system as a mixed waste stream
136. A purge stream comprising non-condensable gases, which may include light impurities derived from col-

EP 0 701 099 B1

umn 50 and redelivered Lo the air separation column 10

via conduit 59, may be withdrawn from condenser 110
via conduit 137 and removed from the system.
[0019] In alternative embodiments, referring still to
Figure 1, a normal purity gaseous nitrogen product may
also be taken from the nitrogen-enriched recycle
stream, preferably derived from a portion of the discharge stream from recycle compressor 60 depicted in
Figure 1 as stream 200. In this embodiment, the remaining portion of the compressed nitrogen-enriched recycle
not taken as normal purity nitrogen product is flowed via
stream 209 to be again cooled and flowed to column 30
as described earlier. In another embodiment, liquid nitrogen product substantially free of heavy contaminants
and light impurities is produced from the bottom of column 50 via line 55 to usage or storage. In any of the
various embodiments depicted in Figure 1, a portion 507
of the intermediate nitrogen-enriched stream 503 free
of heavy contaminants exiting reboiler 90 in column may
be diverted from flowing to column 50 as feed 505, and
instead be cooled and expanded into an upper portion
of the air separation column 10.
[0020] Referring now to the embodiment depicted in
Figure 2, in situations where the nitrogen user requirements do not necessitate substantially complete removal of light impurities, in accordance with further aspects
of the present invention it is possible to produce a nitrogen product substantially free of heavy contaminants,
while containing amounts of light impurities on the order
of the nitrogen-rich stream withdrawn from the main column 10. As depicted in Figure 2, a nitrogen product is
produced directly from the upper portion of the column
10. The process comprises expanding a compressed
and dried feed air stream into an air separation column
to form at the top of the air separation column nitrogenenriched vapor and at the bottom of the air separation
column an oxygen-enriched liquid; withdrawing a portion of the nitrogen-enriched vapor from the air separation column and compressing at least a portion of the
withdrawn portion to an elevated pressure to form an
elevated pressure nitrogen-enriched stream comprising
heavy contaminants; flowing at least a portion of the elevated pressure nitrogen-enriched stream to a second
column wherein heavy contaminants are concentrated
in a bottoms liquid 307 and wherein a nitrogen product
substantially free of heavy contaminants is withdrawn
from the upper portion of the second column. With this
embodiment, the advantages of the embodiments depicted in Figure 1 are retained, while lessening the capital cost associated with a third column.
[0021] Also to provide process flexibility and maintain
efficiency during varying product demands, in further
embodiments, a portion of the cooled feed air flowed to
the main heat exchanger 40 in stream 101 may be diverted from the turbine 80, and instead be further
cooled, and flowed to the column 10 via line 102, and
expanded into the column at an intermediate location,
preferably intermediate in the rectification zone 14. In

this manner, the operating temperature of the expander

can be properly controlled to result in optimum performance.
5

Claims
1.
10

(a) expanding a compressed and dried feed air

stream into an air separation column (10) to
form at the top of the air separation column nitrogen-enriched vapor and at the bottom of the
air separation column an oxygen-enriched liquid;
(b) withdrawing a portion (201) of the nitrogenenriched vapor from the air separation column
and compressing at least a portion of the withdrawn portion to an elevated pressure to form
an elevated pressure nitrogen-enriched product stream comprising heavy contaminants;
(c) flowing at least a portion of the elevated
pressure nitrogen-enriched stream to a second
column (30) wherein heavy contaminants are
concentrated in a bottoms liquid and wherein a
nitrogen vapor substantially free of heavy contaminants is formed in the upper portion of the
second column:
(d) condensing at least a portion of the nitrogen
vapor substantially free of heavy contaminants
against oxygen-enriched liquid by indirect heat
exchange;
(e)recovering as a product at least a portion of
the nitrogen vapor substantially free of heavy
contaminants, characterized in that it comprises withdrawing the portion of the nitrogenenriched vapor at an intermediate location below a vapor-liquid contacting zone (17) of the
air separation column (10) and sending the bottom liquid (307) from the second column to said
intermediate location.

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2.

A process as recited in Claim 1 wherein at least a

portion of the oxygen-enriched liquid is withdrawn
from the air separation column (10), cooled by indirect heat exchange with at least a portion of the
withdrawn nitrogen-enriched stream and utilized to
condense at least a portion of the nitrogen-enriched
vapors at the top of the air separation column in a
condenser (110) to provide reflux for the air separation column.

3.

A process as recited in Claim 1 or 2 wherein the

expansion of the compressed and cooled feed air
is in an expansion turbine (80) from which turbine
at least a portion of the expanded feed air stream

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A process for the production of at least one ultrahigh purity nitrogen product, comprising the steps
of :

EP 0 701 099 B1

(a) einen Strom von verdichteter und getrockneter Einsatzluft in eine Luftzerlegungssule
(10) entspannt, wobei am Kopf der Luftzerlegungssule mit Stickstoff angereicherten
Dampf und im Sumpf der Luftzerlegungssule
mit Sauerstoff angereicherte Flssigkeit anfllt;
(b) einen Teil (201) des mit Stickstoff angereicherten Dampfs aus der Luftzerlegungssule
abzieht und mindestens einen Teil des abgezogenen Teils auf einen erhhten Druck verdichtet, wobei man einen schwere Verunreinigungen enthaltenden, unter erhhtem Druck stehenden, mit Stickstoff angereicherten Produktstrom erhlt;
(c) mindestens einen Teil des unter erhhtem
Druck stehenden, mit Stickstoff angereicherten
Stroms einer zweiten Sule (30) zufhrt, wobei
schwere Verunreinigungen in einer Sumpfflssigkeit konzentriert werden und sich im oberen
Teil der zweiten Sule ein von schweren Verunreinigungen weitgehend freier Stickstoffdampf bildet;
(d) mindestens einen Teil des von schweren
Verunreinigungen weitgehend freien Stickstoffdampfs durch indirekten Wrmeaustausch gegen eine mit Sauerstoff angereicherte Flssigkeit kondensiert;
(e) mindestens einen Teil des von schweren
Verunreinigungen weitgehend freien Stickstoffdampfs als Produkt gewinnt, dadurch gekennzeichnet, da man den Teil des mit Stickstoff
angereicherten Dampfs an einer Zwischenstelle unterhalb einer Dampf-Flssigkeits-Kontaktzone (17) der Luftzerlegungssule (10) abzieht
und die Sumpfflssigkeit (307) aus der zweiten
Sule der Zwischenstelle zufhrt.

is flowed directly to the air separation column.

4.

5.

A process as recited in Claim 3 wherein the operating pressure of the air separation column is at least
20 psi (137.5 kPa) less than the pressure of the second column.
A process as recited in any of Claims 1 to 4 further
comprising further cooling a portion (102) of the
feed air to a temperature less than the temperature
of the portion of the compressed and dried feed air
stream at the inlet to the turbine, and flowing the
further cooled portion to the air separation column
where it is expanded into the column.

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6.

A process to any of Claims 1 to 5 comprising withdrawing a portion of the nitrogen vapor (301) to form
an intermediate stream substantially free of heavy
contaminants and fowing at least a portion of the
intermediate stream to a reboiler (90) positioned below a stripping zone in a third column (50) to provide
boil-up for the third column and thereafter flowing
at least a portion (505) of the intermediate stream
into the third column at a point above the stripping
zone, and withdrawing an ultra-high purity nitrogen
product (55,203) substantially free of light impurities
and heavy contaminants from the third column from
a point below the stripping zone.

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7.

A process as recited in Claim 6 further comprising

producing an ultra-pure liquid nitrogen product (55)
from liquid accumulated in the bottom of the third
column.

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8.

A process as recited in Claims 6 or 7 further comprising cooling at least a portion of the intermediate
stream (301) substantially free of heavy contaminants against at least a portion of the withdrawn nitrogen-enriched stream from the air separation column and flowing the portion (507) of the intermediate stream to the upper portion of the air separation
column (10).

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9.

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10. The process as recited in Claim 6 wherein the operating pressure of the air separation column is between about 3 bar and about 4.5 bar and the pressure of the second column is between about 4 bar
and about 10 bar.

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Patentansprche

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1.

2.

Verfahren nach Anspruch 1, bei dem man mindestens einen Teil der mit Sauerstoff angereicherten
Flssigkeit aus der Luftzerlegungssule (10) abzieht, durch indirekten Wrmeaustausch mit mindestens einem Teil des abgezogenen, mit Stickstoff
angereicherten Stroms abkhlt und zur Kondensation mindestens eines Teils der mit Stickstoff angereicherten Dmpfe am Kopf der Luftzerlegungssule in einem Kondensator (110) zwecks Lieferung
von Rcklauf fr die Luftzerlegungssule verwendet.

3.

Verfahren nach Anspruch 1 oder 2, bei dem man

die Entspannung der verdichteten und abgekhlten
Einsatzluft in einer Entspannungsturbine (80) vornimmt, von welcher mindestens ein Teil des entspannten Einsatzluftstroms direkt der Luftzerlegungssule zugefhrt wird.

4.

Verfahren nach Anspruch 3, bei dem man die Luftzerlegungssule bei einem Arbeitsdruck betreibt,

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A process as recited in Claim 8 wherein the portion

of the intermediate stream is sent to the intermediate location of the air separation column.

Verfahren zur Gewinnung mindestens eines ultrareinen Stickstoffprodukts, bei dem man:

EP 0 701 099 B1

tion comprim et sch dans une colonne de

sparation d'air (10) pour former au sommet de
la colonne de sparation d'air une vapeur enrichie en azote et au fonds de la colonne de sparation d'air, un liquide enrichi en oxygne ;
(b) de retrait d'une portion (201) de la vapeur
enrichie en azote de la colonne de sparation
d'air et de compression d'au moins une portion
de la portion retire une pression leve pour
former un courant de produit enrichi en azote
pression leve comprenant des contaminants
lourds ;
(c) d'coulement d'au moins une portion du
courant de produit enrichi en azote pression
leve vers une deuxime colonne (30), dans
laquelle les contaminants lourds sont concentrs dans un liquide de fond et dans laquelle
une vapeur d'azote substantiellement exempte
de contaminants lourds est forme dans la portion suprieure de la deuxime colonne ;
(d) de condensation d'au moins une portion de
la vapeur d'azote substantiellement exempte
de contaminants lourds contre-courant du liquide enrichi en oxygne par change thermique indirect ;
(e) de rcupration en tant que produit d'au
moins une portion de la vapeur d'azote substantiellement exempte de contaminants lourds,
caractris en ce qu'il inclut le retrait de la portion de vapeur enrichie en azote un emplacement intermdiaire en dessous de la zone de
contact liquide-vapeur (17) de la colonne de sparation d'air (10) et d'envoi du liquide de fond
(307) de la deuxime colonne audit emplacement intermdiaire.

der mindestens 20 psi (137,5 kPa) unter dem Druck

der zweiten Sule liegt.
5.

6.

7.

8.

9.

Verfahren nach einem der Ansprche 1 bis 4, bei

dem man ferner eine Teil (102) der Einsatzluft auf
eine unter der Temperatur des Teils des Stroms von
verdichteter und getrockneter Einsatzluft am Eingang der Turbine liegende Temperatur abkhlt und
den weiter abgekhlten Teil der Luftzerlegungssule zufhrt und in die Sule entspannt.
Verfahren nach einem der Ansprche 1 bis 5, bei
dem man einen Teil des Stickstoffdampfs (301) abzieht, wobei man einen von schweren Verunreinigungen weitgehend freien Zwischenstrom erhlt
und mindestens einen Teil des Zwischenstroms einem unterhalb einer Abtriebszone in einer dritten
Sule (50) angeordneten Verdampfer (90) zwecks
Lieferung von Verdampfungsanteil fr die dritte
Sule zufhrt und danach mindestens einen Teil
(505) des Zwischenstroms an einem Punkt oberhalb der Abtriebszone der dritten Sule zufhrt und
aus der dritten Sule an einem Punkt unterhalb der
Abtriebszone ein von leichten und schweren Verunreinigungen weitgehend freies ultrareines Stickstoffprodukt (55, 203) abzieht.
Verfahren nach Anspruch 6, bei dem man ferner
aus Flssigkeit, die sich im Sumpf der dritten Sule
gesammelt hat, ein ultrareines flssiges Stickstoffprodukt (55) gewinnt.
Verfahren nach Anspruch 6 oder 7, bei dem man
ferner mindestens einen Teil des von schweren Verunreinigungen weitgehend freien Zwischenstroms
(301) gegen mindestens einen Teil des aus der Luftzerlegungssule abgezogenen, mit Stickstoff angereicherten Stroms abkhlt und den Teil (507) des
Zwischenstroms dem oberen Teil der Luftzerlegungssule (10) zufhrt.

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2.

Procd selon la revendication 1, caractris en

ce qu'au moins une portion du liquide enrichi en
oxygne est retire de ladite colonne de sparation
d'air (10), refroidie par change thermique indirect
avec au moins une portion du courant retir enrichi
en azote et utilise pour condenser au moins une
portion des vapeurs enrichies en azote au sommet
de la colonne de sparation d'air dans un condenseur (110) pour fournir un reflux pour la colonne de
sparation d'air.

3.

Procd selon la revendication 1 ou 2, caractris

en ce que la dtente de l'air aliment comprim et
refroidi se passe dans une turbine de dtente (80),
partir de laquelle au moins une portion du courant
d'air d'alimentation dtendu s'coule directement
vers la colonne de sparation d'air.

4.

Procd selon la revendication 3, caractris en

ce que la pression opratoire de la colonne de sparation d'air est au moins infrieure de 20 psi
(137,5 kPa) la pression de la deuxime colonne.

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Verfahren nach Anspruch 8, bei dem man den Teil

des Zwischenstroms der Zwischenstelle der Luftzerlegungssule zufhrt.
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10. Verfahren nach Anspruch 6, bei dem man die Luftzerlegungssule bei einem Arbeitsdruck zwischen
etwa 3 bar und etwa 4,5 bar und die zweite Sule
bei einem Druck zwischen etwa 4 bar und etwa 10
bar betreibt.

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Revendications
1.

Procd de production d'au moins un produit d'azote puret ultra leve, comprenant les tapes :

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(a) d'expansion d'un courant d'air d'alimenta-

10

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5.

EP 0 701 099 B1

Procd selon l'une quelconque des revendications

1 4, comprenant en outre le refroidissement supplmentaire d'une portion (102) de l'air d'alimentation une temprature infrieure la temprature
de la portion du courant d'air d'alimentation comprim et sch l'entre de la turbine, et l'coulement
de la portion refroidie supplmentaire vers la colonne de sparation d'air o elle est dtendue dans la
colonne.

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6.

7.

8.

9.

Procd selon l'une quelconque des revendications

1 5, comprenant le retrait d'une portion de la vapeur d'azote (301) pour former un courant intermdiaire substantiellement exempt de contaminants
lourds et l'coulement d'au moins une portion du
courant intermdiaire vers un rebouilleur (90) dispos en dessous d'une zone de stripping dans une
troisime colonne (50) pour fournir un taux de revaporisation pour la troisime colonne et, par la suite
l'coulement d'au moins une portion (505) du courant intermdiaire dans la troisime colonne en un
point au-dessus de la zone de stripping, et le retrait
d'un produit d'azote puret ultra leve (55, 203),
substantiellement exempt d'impurets lgres et de
contaminants lourds en provenance de la troisime
colonne d'un point en dessous de la zone de stripping.
Procd selon la revendication 6, comprenant en
outre la production d'un produit d'azote liquide ultra
pure (55) partir du liquide accumul dans le fond
de la troisime colonne.
Procd selon les revendications 6 ou 7, comprenant en outre le refroidissement d'au moins une portion du courant intermdiaire (301), substantiellement exempt de contaminants lourds contre-courant d'au moins une portion retire du courant enrichi en azote provenant de la colonne de sparation
d'air et l'coulement de la portion (507) du courant
intermdiaire la portion suprieure de la colonne
de sparation d'air (10).
Procd selon la revendication 8, caractris en
ce que la portion du courant intermdiaire est envoye l'emplacement intermdiaire de la colonne
de sparation d'air.

10. Procd selon la revendication 6, caractris en

ce que la pression opratoire de la colonne de sparation d'air est comprise entre environ 3 bars et
environ 4,5 bars et en ce que la pression de la
deuxime colonne est comprise entre environ 4
bars et environ 10 bars.

15

20

25

30

35

40

45

50

55

12

EP 0 701 099 B1

EP 0 701 099 B1