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Patent 2159308 Summary

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(12) Patent Application: (11) CA 2159308
(54) English Title: AIR SEPARATION METHOD AND APPARATUS TO PRODUCE NITROGEN
(54) French Title: METHODE ET APPAREIL POUR L'OBTENTION D'AZOTE PAR EXTRACTION DE L'AIR
Status: Deemed Abandoned and Beyond the Period of Reinstatement - Pending Response to Notice of Disregarded Communication
Bibliographic Data
(51) International Patent Classification (IPC):
  • F25J 3/04 (2006.01)
(72) Inventors :
  • MOSTELLO, ROBERT A. (United States of America)
(73) Owners :
  • THE BOC GROUP, INC.
(71) Applicants :
  • THE BOC GROUP, INC. (United States of America)
(74) Agent: GOWLING WLG (CANADA) LLP
(74) Associate agent:
(45) Issued:
(22) Filed Date: 1995-09-27
(41) Open to Public Inspection: 1996-04-26
Examination requested: 1995-09-27
Availability of licence: N/A
Dedicated to the Public: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data:
Application No. Country/Territory Date
08/329,035 (United States of America) 1994-10-25
08/374,060 (United States of America) 1995-01-19
08/459,946 (United States of America) 1995-05-31

Abstracts

English Abstract


An air separation method and apparatus for producing nitrogen is provided in
which oxygen enriched liquid, produced as a column bottoms of a distillation column, is
partially vaporized and phase separated. The vapor phase is expanded to provide
refrigeration while the liquid phase, after pressure reduction, is introduced into the head
condenser to condense reflux to the column. Alternatively, part of the oxygen enriched
liquid can be fully vaporized and then expanded to provide refrigeration. In such case,
another part of the oxygen enriched liquid can be used to condense reflux to the column.
Part of the air to be separated is liquefied against the oxygen enriched liquid to be
vaporized and then introduced into a lower portion of the column to maintain production
and purity levels that would have been obtained had all the oxygen enriched liquid stream
been used in condensing reflux to the column.


Claims

Note: Claims are shown in the official language in which they were submitted.


I Claim:
1. A method of separating air to produce a nitrogen product comprising:
separating the air by a low temperature rectification process employing a
distillation column to produce an oxygen rich liquid column bottoms and a nitrogen rich
vapor tower overhead and a head condenser to condense at least part of the nitrogen rich
vapor tower overhead to reflux said distillation column;
said low temperature rectification process including:
partially vaporizing an oxygen enriched liquid stream composed of said
oxygen rich liquid column bottoms;
separating said oxygen enriched liquid stream into liquid and vapor phases;
expanding a liquid phase stream composed of the liquid phase to create a
temperature difference between said liquid phase stream and said nitrogen rich vapor
tower overhead and introducing said liquid phase stream as a coolant stream into said
head condenser so that heat is transferred from said at least part of the nitrogen rich vapor
to said coolant stream thereby causing said condensation of said at least part of said
nitrogen rich vapor tower overhead;
expanding a vapor phase stream composed of the vapor phase with the
performance of work to produce a refrigerant stream utilized to at least partially
refrigerate said low temperature rectification process; and
extracting a product stream from a remaining part of said nitrogen rich
vapor tower overhead not utilized in said distillation column as said reflux to form said
nitrogen product.

2. The method of claim 1, wherein:
said oxygen enriched liquid stream is partially vaporized by indirectly exchanging heat
with part of the air to be separated, thereby causing said part of the air to be separated
to liquefy;
said part of the air to be separated is introduced into said distillation column as
intermediate reflux to maintain production of said product stream at a level that would
have been obtained had the entire oxygen enriched liquid stream been utilized to condense
said at least part of said nitrogen rich vapor tower overhead; and
prior to said partial vaporization of said oxygen enriched liquid stream, said oxygen
enriched liquid stream is expanded to produce a temperature difference for said indirect
heat exchange between said part of said air and said oxygen enriched liquid stream.
3. The method of claim 2, further comprising:
removing a vapor stream from said distillation column;
condensing said vapor stream by indirectly exchanging further heat between said vapor
stream and said oxygen enriched stream; and
introducing said vapor stream back into said distillation column, above said intermediate
reflux, as additional reflux.
4. A method of separating air to produce a nitrogen product comprising:
separating the air by a low temperature rectification process employing a
distillation column to produce an oxygen rich liquid column bottoms and a nitrogen rich
vapor tower overhead and a head condenser to condense at least part of the nitrogen rich
vapor tower overhead to reflux said distillation column;
16

said low temperature rectification process including:
dividing an oxygen enriched liquid stream composed of said oxygen rich
liquid column bottoms into first and second partial streams;
expanding said first partial stream to create a temperature difference
between said first partial stream and said nitrogen rich vapor tower overhead and
introducing said first partial stream as a coolant stream into said head condenser so that
heat is transferred from said at least part of the nitrogen rich vapor to said coolant stream
thereby causing said condensation of said at least part of said nitrogen rich vapor tower
overhead;
vaporizing said second partial stream;
expanding said second partial stream with the performance of work to
produce a refrigerant stream utilized to at least partially refrigerate said low temperature
rectification process; and
extracting a product stream from a remaining part of said nitrogen rich
vapor tower overhead not utilized in said distillation column as said reflux to form said
nitrogen product.
5. The method of claim 4, wherein:
said second partial stream is vaporized by indirectly exchanging heat with part of
the air to be separated, thereby causing said part of the air to be separated to liquefy;
said part of the air to be separated is introduced into said distillation column as
intermediate reflux to maintain production of said product stream at a level that would
have been obtained had an amount of flow equal to both said first and second partial
17

streams been utilized to condense said at least part of said nitrogen rich vapor tower
overhead; and
prior to said vaporization of said second partial stream, said second partial stream
is expanded to produce a temperature difference for said indirect heat exchange between
said part of said air and said second partial stream.
6. The method of claim 5, further comprising:
removing a vapor stream from said distillation column;
condensing said vapor stream by indirectly exchanging further heat between said vapor
stream and said second partial stream; and
introducing said vapor stream back into said distillation column, above said intermediate
reflux, as additional reflux.
7. The method of claim 3 or claim 6, wherein:
said oxygen enriched liquid stream is subcooled within a subcooling unit prior to
being partially vaporized;
said heat transfer to said coolant stream vaporizes said coolant stream to form a
vaporized coolant stream;
said air to be separated is divided into first and second subsidiary streams;
said first subsidiary stream is introduced into said distillation column;
said second subsidiary stream forms said part of said air to be separated;
18

said oxygen enriched stream is subcooled through additional heat exchange with
said refrigerant stream, said product stream, and said vaporized coolant stream within a
subcooling unit; and
said refrigerant, vaporized coolant and said product streams are partially warmed
within said subcooling unit and are then fully warmed.
8. An apparatus for separating air to produce a nitrogen product, said apparatus
comprising:
a filter for filtering the air;
a compressor connected to the filter for compressing the air;
an after-cooler for removing heat of compression from the air;
a pre-purification unit for purifying the air;
main heat exchange means for cooling the air to a temperature suitable for its
rectification;
a distillation column configured to rectify the air into an oxygen rich liquid column
bottoms and a nitrogen rich vapor tower overhead;
a head condenser connected to said distillation column to condense at least part of the
nitrogen rich vapor tower overhead to reflux said distillation column;
vaporization means for partially vaporizing an oxygen enriched liquid stream composed
of said oxygen enriched liquid column bottoms;
19

a phase separator connected to said vaporization means for separating said oxygen
enriched liquid stream into liquid and vapor phases;
said phase separator connected to said head condenser so that heat is transferred from said
at least part of the nitrogen rich vapor to a coolant stream made up of a liquid phase
stream composed of said liquid phase, thereby causing said condensation of said at least
part of said nitrogen rich vapor tower overhead and vaporization of said coolant stream
to form a vaporized coolant stream;
a pressure reduction valve interposed between said phase separator and said head
condenser to expand said liquid phase stream and thereby create said coolant stream and
a temperature difference between said coolant stream and said nitrogen rich vapor tower
overhead;
said phase separator also connected to said main heat exchange means so that a vapor
phase stream composed of said vapor phase partially warms;
expansion means connected to said main heat exchange means for expanding said vapor
phase stream with the performance of work to produce a refrigerant stream;
said main heat exchange means in communication with said expansion means so that said
refrigerant stream fully warms within said main heat exchange means;
means for extracting a product stream composed of a remaining part of said nitrogen rich
vapor tower overhead not utilized in said distillation column as said reflux to form said
nitrogen product; and
said main heat exchange means connected to said product stream extracting means so that
said product stream fully warms within said main heat exchange means.
9. The apparatus of claim 8, wherein:

said vaporization means is connected to said main heat exchange means and has means
for indirectly exchanging heat between said oxygen enriched liquid stream and said part
of said air to be separated so that said oxygen enriched liquid stream is partially vaporized
and said part of the air to be separated liquefies and a first pressure reduction valve
configured to expand said oxygen enriched liquid stream to produce a temperature
difference for said indirect heat exchange between said part of said air and said oxygen
enriched liquid stream;
said pressure reduction valve interposed between said phase separator and said head
condenser constituting a second pressure reduction valve; and
said vaporization means is connected to said distillation column so that said part of the
sir to be separated is introduced into said distillation column as intermediate reflux to
maintain production of said product stream at a level that would have been obtained had
the entire oxygen rich liquid stream been utilized to condense said at least part of said
nitrogen rich vapor tower overhead.
10. The apparatus of claim 9, further comprising said vaporization means also having
means for indirectly exchanging further heat between a vapor stream and said oxygen rich
liquid stream so that said vapor stream condenses and said vaporization means connected
to said distillation column so that said vapor stream flows from said distillation column
into said vaporization means and thereafter returns to said distillation column, above said
intermediate reflux, as additional reflux.
11. An apparatus for separating air to produce a nitrogen product, said apparatus
comprising:
a filter for filtering the air;
a compressor connected to the filter for compressing the air;
21

an after-cooler for removing heat of compression from the air;
a pre-purification unit for purifying the air;
main heat exchange means for cooling the air to a temperature suitable for its
rectification;
a distillation column configured to rectify the air into an oxygen rich liquid column
bottoms and a nitrogen rich vapor tower overhead;
a head condenser connected to said distillation column for condensing at least part
of the nitrogen rich vapor tower overhead to reflux said distillation column against
vaporizating a coolant stream made up of a first partial stream composed of said oxygen
rich liquid column bottoms, thereby to form a vaporized coolant stream;
a pressure reduction valve connected to said head condenser to expand said first
partial stream and thereby to create said coolant stream and a temperature difference
between said coolant stream and said nitrogen rich vapor tower overhead;
vaporization means for vaporizing a second partial stream composed of said
oxygen rich liquid column bottoms;
said vaporization means connected to said main heat exchange means so that said
second partial stream partially warms;
expansion means connected to said main heat exchange means for expanding said
second partial stream with the performance of work to produce a refrigerant stream;
said main heat exchange means in communication with said expansion means so
that said refrigerant stream fully warms within said main heat exchange means;
22

means for extracting a product stream composed of a remaining part of said
nitrogen rich vapor tower overhead not utilized in said distillation column as said reflux
to form said nitrogen product; and
said main heat exchange means connected to said product stream extracting means
so that said product stream fully warms within said main heat exchange means.
12. The apparatus of claim 11, wherein:
said vaporization means is connected to said main heat exchange means and has
means for indirectly exchanging heat between said second partial stream and a part of said
air to be separated so that said second partial steam is vaporized and said part of the air
to be separated liquefies and a first pressure reduction valve configured to expand said
second partial stream to produce a temperature difference for said indirect heat exchange
between said part of said air and said second partial stream;
said pressure reduction valve interposed between said sub-cooling unit and said
head condenser constitutes a second pressure reduction valve; and
said vaporization means is connected to said distillation column so that said part
of the air to be separated is introduced into said distillation column as intermediate reflux
to maintain production of said product stream at a level that would have been obtained
had an amount of flow equal to said first and second partial streams been utilized to
condense said at least part of said nitrogen rich vapor tower overhead.
13. The apparatus of claim 12, further comprising said vaporization means also having
means for indirectly exchanging further heat between a vapor stream and said second
partial stream so that said vapor stream condenses and said vaporization means connected
to said distillation column so that said vapor stream flows from said distillation column
into said vaporization means and thereafter returns to said distillation column, above said
intermediate reflux, as additional reflux.
23

14. The apparatus of claim 8 or claim 11, further comprising:
a subcooling unit interposed between said distillation column and said head
condenser for subcooling said oxygen enriched liquid stream;
a junction connected to said heat exchange means so that said air to be separated
is divided into first and second subsidiary streams;
said junction connected to said distillation column so that said first subsidiary
stream flows into said distillation column and said junction also connected to vaporization
means so that said part of said air to be separated is formed by said second subsidiary
stream; and
said main heat exchange means configured for fully warming said refrigerant,
vaporized coolant and said product streams and connected to said subcooling unit so that
said refrigerant, vaporized coolant and said product streams partially warm within said
subcooling unit and then fully warm therewithin.
24

Description

Note: Descriptions are shown in the official language in which they were submitted.


- 2159308
AIR SEPA~TION METHOD AND APPARATUS TO PRODUCE NITROGEN
p~FT A.TFn APPT ~CAT~ONS
lhis is a co~ t;on-in-part of U.S. Patent Application 08/374,060 filed ~anuary
19, 1995, which was a co~ aLion-in-part of 08/329,035 filed October 25, 1994.
RACKGROUNn OF THF INVFNTION
The present invention relates to a method of sepalatillg air by a low te~lpe.al~lre
rectification process employing a ~iicti~ on column to produce a nitrogen product. More
particul~rly, the present invention relates to such a method and a~p~al~s in which a
portion of oxygen enriched liquid produced as a column bottoms in the ~lictill~tion column
S vaponzed and then c~p~ndPd to supply refrigeration and another portion of the oxygen
enriched liquid, after eXp~ncion~ is used to c~dPnce nitrogen vapor in a head c~ndencPr
~tt~rhPd to the distillation column. Even more particularly, the present invention relates
to such a method and app~allls in which the portion of the oxygen enriched liquid is
vaporized by a part of the inr~ming air and under certain conditions an additional
10 condencing stream of lesser oxygen content than air withdrawn from the tlictill~tion
column. The part of inComing air and the additional cond,oncinp strearn are thereby
liquefied and introduced into the column as additional reflux streams to m~int~in the rate
and/or concenL~alion of nitrogen production to prior art levels.
Nitrogen is produced by low telll~.dl~ rectification of the air in an air sep ation
plant. Often such plants employ a single ~ictill~tion column and are known in the art as
Ditrogen generators. After air has been filtered, collll,lesscd and purified, the air is cooled
to a tc~ a~ suitable for its rectification. This te.,l~ldl lre is norrnally at or near the
dew point of the air. Thereafter, the air is introduced into a distillation column having
20 liquid-vapor contarting elements which can be forrned by trays and/or paC~inec~ either
structured or random. In the distillation column an ~cc~n~ing vapor phase of the air is

~159~08
cont~ ted by a descendinp liquid phase. The result of such cont~ct is that the liquid phace
becoll,es cve~nore concen~aled in oxygen to produce a oxygen enriched liquid column
bottoms and the PCc~ ing vapor phase becollles eve~nore concentrated in nitrogen to
produce a nitrogen rich ~-apor tower overhead.
ln order to reflux the column, a head condenser is provided in which the nitrogen
vapor tower overhead is partially condence~ The con~lPnc~e is retumed to the rli~till~tion
column as reflux. Typically, an oxygen cnriched liquid stream composed of the column
bottoms is ~ lo~ed, exr~r~ded to a low ~Il~.a~lre, and then introduced as the coolant
10 for the head condenser. The product is removed from the top region of the column
mostly as a vapor.
ln any type of air separation plant, there is ~lltillual heat leakage into the plant
and enthalpy differences bel..~en the air feed and product streams at the warm end of the
lS plant. Such heat leakage ll~lileS refrigeration to bc supplied to the air separation plant.
If the nitrogen product is to be rn~in1~in~Pd at column pressure, refrigeration is generally
supplied from outside the column envelope. Work expansion obtained from the vaporized
oxygen enriched liquid, all of which is vaporized in the head conflencpr~ or by exp~nding
air from a higher pressure down to column pressure are usual methods of supplying
20 refrigeration. There are also "liquid assist plants" in which liquid nitrogen is added to the
column from an external source in order to supply the requisite refrigeration.
As will be ~ cu~se~l the present invention relates to an air separation technique
in which refrigcration is generated in a manner that rcduces the cnergy PYpen~iture in
2S producing a nitrogen product This is Aec4...plished by more efficiently using energy for
air separation and making cnergy, folll,elly in excess, available for refrigeration.
SUMM~Y OF THF lNVF~llON
The present invention provides a method of separating air to produce a nitrogen
product. In accordance with the method, the air is separated by a low te~ re

- 2~59308
rectification process employing a tlictill~tion column to produce an oxygen rich liquid
column bottoms and a nitrogen rich vapor tower overhead. A head condenser is provided
to condense at least part of the nitrogen rich vapor tower overhead to reflux the
till~tion column.
In one aspect of the present invention, the low te~pe.dlulc rectification process
includes partially vaporizing an oxygen enriched liquid stream composed of the oxygen
rich liquid column bottoms. The oxygen enriched liquid s~eam is thereaRer separated
into liquid and vapor phases and a liquid phase stream composed of the liquid phase is
10 expanded to create a tc~ a~ difference between the liquid phase stream and the
nitrogen rich vapor tower overhead. The liquid phase stream is introduced into the head
condenser as a coolant stream so thdt heat is transferred from the at least part of the
nitrogen rich vapor to the coolant stredm to thereby cause the condenc~tion of the at least
part of the nitrogen rich vapor tower overhead. A vapor phase stream, composed of the
15 vapor phase is exr~nded with the performance of work to produce a refrigerant stream
utilizèd to at least partially refrigerate the low tem~.dl~re rectification process. A
product stream is extracted from a rem~inin~ part of the nitrogen rich vapor tower
overhead, not utilized in the llictill~tion column as the reflux, to form the nitrogen product.
In another aspect ofthe present invention, the low te~,dtLlre rectification process
includes dividing an oxygen enriched liquid stream composed of the oxygen rich liquid
column bottoms into first and second partial streams. The first partial stream is exr~n~ed
to create a tell~pela~lre difference between the first partial stream and the nitrogen rich
vapor tower overhead. The first partial stream is introduced as a coolant stream into the
head condenser so that heat is ~arLferred from the at least part of ~e nitrogen rich vapor
to the coolant stream thereby c~lcing condenc~tion of the at least part of the nitrogen rich
vapor tower ov~rhead. The æcond partial stream is ~a~l~d and then partially warrned
aflLer having been vaporized. The second par~al stream is eYI-~nded with the ~,~l~lance
of work to produce a refrigerant stream utilized at least to partially refrigerate the low
tcll~clal~lre rèctification process. A product stream is extracted from a rem~ining part of

~lS9308
the nitrogen rich vapor tower overhead not utiliæd in the distillation column as the reflux
to form the nitrogen product.
The present invendon also provides an a~p~alus for S~alil~g air to produce a
S nitrogen product. In accordance with the app~allls~ a filter is provided for filtering the
ur and a CClllpleSSOl iS col~l.P~t ~ to the filter for co~plescing ~e ur. An after-cooler
is provided for removing heat of co~ ,lession from the air and a pre-purification unit is
provided for punfying the air. A rnain heat exchAnee means cools the air to a te~ al~e
suitable for its rectification uld a lictillAtioD column is configured to rectify the air into
10 an oxygen rich liquid column bottoms and a nitrogen rich vapor tower overhead. A head
condenser is connected to the Aictill~tion column to c~ence at least part of the nitrogen
rich vapor tower overhead for reflux to the Aictill~tion column.
In accordance with a further aspect of the present invention, a vaporization means
15 is col-~.ecle~ to the lictillAtion column for partially vaporizing an oxygen enriched liquid
stream composed of the oxygen rich liquid column bottoms and a phase separator is
conn~ cted to the vaporization means for sepa.ating the oxygen enriched liquid strearn into
liquid and vapor phases. The phase sep rator is connP~led to the head co~dencer so that
heat is transferred from the at least part of the nitrogen rich vapor to a coolant stream
20 made up of a liquid phase strearn composed of the liquid phase. The result is to cause
con~nc~tion of the at least part of the nitrogen rich vapor tower overhead and
vaporization of the coolant stream to form a vapo,.2~d coolant stream th~lcf~om. A
~leaàu,c reduction valve is interposed between the phase separator and the head con~ncer
to cxpand the liquid phase stream and thereby create the coolant stream and a t~ lu,e
25 difI~.e.,ce between the coolant stream and the nitrogen rich vapor tower ovahead. The
phase separator is also con~ t~ to the main heat PYrh~nee means so that the vapor
phase stream co..,posed of the vapor phase partially wa~ns. An expansion means is
connected to the main heat exchange means for eyr~n~ine the vapor phase strearn with
the performance of work to produce a refrigerant strearn. The main heat exchange m~nc
30 is in comrnunication with the expansion means so that the refrigerant strearn fully warrns
within the main heat exchange means. A means is provided for extracting a product

- - 2159308
stream composed of a rem~inin~ part of the nitrogen rich vapor tower overhead, not
utilized in the tlictill~tion column as the reflux, to forrn the nitrogen product and the main
heat exchange means is connP~l~d to the product stream cxtracting means so that the
product stream fully warms within the main heat exchange means.
S
In accordance with a still further aspect of the present invention, the head
conden~er is connl~c~ed to the (lictill~tion colllmn so that heat is transferred from the at
least part of the nitrogen rich vapor to a coolant st~earn made up of a firct partial stream
composed of the oxygen rich liquid colurnn bottorns. This causes the contlen~tion of the
10 least part of the nitrogen rich vapor tower overhead and vaporization of the coolant stream
to form a vaporized coolant stream. A pressu,e reduction valve is interposed between the
~ictill~tion column and the head condenser to expand the fir t partia] stream and thereby
create the coolant stream and a te~latule difference between the coolant stream and the
rlitrogen rich vapor tower overhead. A vaporization means is conn~cted to the ~ictill~tion
15 column for vaporizing a second partial strearn ~.ll~osed ofthe oxygen rich liquid column
bottoms. The vaporization means is also com~ ed to the main heat exchange means so
that the second partial strearn partially warms. An expansion meanc is conn~cted to the
main heat exchange means for expanding the second partial stream with the performance
of work to produce a refrigerant strearn. The main heat exchange means is in
20 cornmunication with the exparlsion means so that the refrigerant stTeam fillly warms
within the main heat cxchange means. A means is provided for extracting a product
stream composed of the reTn~ining part of the nitrogen rich vapor tower overhead not
utilized in the dictill~tion colurnn as the reflux to form the nitrogen product. The main
heat ~xch~n~e means is also connecl~ to the product stream extracting means so that the
25 product stream fully warms within the meat exrh~nge means.
The present invention functions by talcing advantage of the larger-than-nPc~s~ ydriving forces that are employed in the ~ tjoD of air to create the nitrogen product.
In the present inven~ion, the oxygen enriched liquid acts as a coolant for con~en~ing
30 reflux to the column and serves to supply at least part of the refrigeration needs of the
plant, independent of aforementioned typical refrigeration processes

~15 9308
Since not all of the oxygen cnriched liquid is being utilized in a reflux
condencAtion role, there is potentially an insufflcient supply of reflux produced by the
head condenser. In order to co~ e for such reduced reflux production, intermediate
reflux can be supplie~, at the vcry least, by liquid air and ~.efc.e..tially by both liquid air
5 and another reflux stream of lesser oxygen content than air. Thus, in yet still another
aspect, thc present invention enco...~ ~s a method in which the oxygen cnriched liquid
stream or a part thereof is partially or wholly vaporized by indirectly ~xch~nging heat
with part of the air to bc separated and preferably, with another vapor stream withdrawn
from the column of lesser oxygen content than air, thereby callcing the part of the air to
10 be separated and if present, the other vapor strearn to liquefy. The part of the air to be
separated and preferably, the other liquefied vapor strearn withdrawn from the colurnn are
then introduced into the dictil~tion column as i~ ,...r~;~te reflux streams to m~int~in
production of the product strearn at a level that would have been obtained had the entire
oxygen rich liquid stream been utilized to condense the at leact part of the nitrogen rich
15 vapor tower o~. lLead. Prior to the partial ~a~.i~alion of the oxygen rich liquid stream
or the complete vapol~ion of part of the oxygen enrich liquid stream, the oxygenenriched liquid is eYp~ e~ to produce a te~lalule difference for the indirect heat
eYch~nge with the part of the air and preferably, if present, the vapor strearn withdrawn
from the column.
nFSCRTPTlON OF THF nRA~lING
While the specification concludes with claims distinctly pointing out the subject
matt that Applicant regards as his invention, it is believed the invention will be better
2~ understood when taken in com1e~lion with the ~ ...p~-ying drawing in which:
Fig. 1 is a sch~m~tic illustration of an air separation plant ope.dtiilg in accordance
with a method and a~p~al~s of the present invention; and

2159308
Fig. 2 is an altemative embodiment of Fig. 1. In order to avoid needless repetition
in the explanation of Fig. 2, the numbering scheme used in Fig. I is carried over to Fig.
2 for co,llponents and streams tht share common function.
nFT,~TT.F.n nF,SCRTPTION
With ,~fe.ence to Fig. 1, a single column nitrogen generator 10 is illustrated. An
~c~ing air strearn 12 is filtered by a filter 14 to remove dust particles and the like. Air
stream 12, after having been filtered7 is coll~ ess~d by a colllplessor 16 and thereafter,
10 the heat of colllpless;on is removed by a conventional after-cooler 18. Water, carbon
dioxide and heavy trace colllponents of the air such as hydrocarbons are removed by a
pre-purification unit 20 conn~cted to aftercooler 18. Pre-purification unit 20 can comprise
several beds of adsorbent o~,~Ling out of phase for regeneration purposes.
Air stream 12 having thus been filtered and purified is then introduced into a main
heat eyrh~nger 22. The air to be separated enters main heat exçh~n~er 22 and is then
fully cooled to a temp~ suitable for its rectification. In this regard, the term "fully
cooled" as used herein and in the claims means cooled to a te.llpe,alule at which the
rectification is conduct~ The tcrm "fully warmed" as used herein and in the claims
means warrned to a telllpe~atulc of the warm end of main heat exchanger 22. The term
"partially warrned" meanc warmed to a temperature above the rectification te.ll~,al lre
but below the telllpelal~e of the warrn end of main heat exchanger 22.
After having been fully cooled within main heat exch~nPer 22, air stream 12 is
then divided into first and second subsidiary streams 24 and 26 ~s~cti~ely. A junction,
fo~med by T-sections of pipe, headers and the like, is co.-..ccted to main heat eYrh~nger
for this ~ ose. First subsidiary stream 24 co~slituhs a major portion of the air to be
separated and is introduced into a single ~ tillAtion column 30 which is provided by
liquid-vapor co~t~rting elements 32, 34 and 36 which can be trays and/or structured
30 p~r~in~, random p~c~ing and etc. Distillation column 30 rectifies the incoming air into
an oxygen rich liquid column bottoms that collects within bottom region 38 of distillation

- ~159308
column 30 and a rlitrogen rich vapor tower overhead which collects in a top region 40 of
distillation column 30. A head condenser 42 is connect~Pd to tlictill~tion column 30 to
condPnce at least part of the nitrogen rich vapor tower overhead collected in top region
40 of ~ictill~tion column 30. To this cnd, part of a nitrogen vapor stream 44 is cxtracted
5 from top region 40 of listill~tion column 30 and is introduced into head cor ~enCpr 42.
Nitrogen vapor stream 44 is in part cond~pnce~ by a coolant s$ream 46, which in turn
~a~o~ s to produce a va~ol;~d coolant strearn 47. After c~n~Pn~tion~ nitrogen vapor
stream 44 is ~ ed as a reflux stream 48 and to top region 40 of ~ictill~tion column 30.
An oxygen enriched liquid stream 50, composed ofthe oxygen rich liquid column
bonoms, is extracted from bottom region 38 of iictill~tion column 30. Oxygen enriched
liquid stream 50 can then be preferably subcooled within a subcooler unit 52 to minimi7P
vapor formation upon subsequent valve expansion. Thereafter, oxygen cnriched liquid
stream 50 is partially va~olized within a vaporizer 54 after having passed through a
15 ples~ reduction valve 55 (described in more detail hereinafter) and then introduced into
a phase se~a~or 56 to separate oxygen enriched liquid s$ream 50 into liquid and vapor
phases.
A liquid phase stream 58 colllposed of the liquid phase is extracted from phase
20 separator 56 and is then passed through a pres~ule reduction valve 60 to sufficiently lower
the t~,ll~,al~lre of liquid phase stream 58 that it can serve as the coolant for head
condenser 42. Thus, liquid phase stream 58 after passage through plC5~Llle reduction
valve 60 is converted into coolant stream 46 which has been dicc~lcsed hereinabove.
Phace separator 56 is also conn~le~d to the main heat exch~nger 22 so that a vapor
phase stream 62, cu~ os~ of the vapor phase, partially wa~ns within main heat
e~k~ .~e~ 22. Vapor phase stream 62 af~er having been partially warmed is exr~nde~ in
a ~ der 64 or other cxpansion m~chin~ connPc1ed to main he~at exch~n~er 22.
The expansion ûf vapor phase strearn 62 produces a refrigerant strearn 66.

2159308
In the illustrated embodi~nent, re~igerant strearn 66 also partially warms within
subcooler unit 52 as does vaporized coolant strearn 47 and a product stream 68. As
illustrated, vaporized coolant strearn 47, aRer subcooler unit 52, fillly wanns within main
beat exr-h~nPer 22 to form a waste nitrogen stream labelled WN~. Part of warrn vaporized
5 coolant stream 47 can be fed to pre-purification unit 20 for bed 1~ gene.aLion purposes.
Main heat eYr-h~nper 22 is in co~ul~ication with turboeYr~n-ler 64 so that refrigerant
stream 66 cventually fillly warms within main heat cyr~n-er 22 and is discha~ged as a
waste st~eam, desigr ~tcd as WN2. A product strcam 68 is formed which is con~posed of
the nitrogen vapor tower overhead collected in top region 40 of ~ictill3tion column 30.
10 Product stream 68 co~liLuLes a reTn~ining portion of the nitrogen vapor tower overhead
that is not used in fo~ming reflux to ~lictill~tion column 30. After partial warming in
subcooling unit 52, product strearn 68 fuIly warms within main heat eY~h~nger 22 and is
discharged as a product stream, labelled PN. Against the partial wam~ing of the foregoing
mentioned steams, as mentioned previously, oxygen enriched liquid strearn 50 subcools.
In single col-~mn nitrogen generator 10 oxygen enriched liquid strearn 50 is
partially vaporized in vaporizer 54 and thus, only part of oxygen enriched liquid stream
50 is used as coolant for head conden~r 42. As a result, there is less reflux contributed
through condenc~tion of tower overhead in single colu nn nitrogen generator 10 than in
20 a nitrogen generator of the prior art. If no other reflux were added (an operation
col-t~.,.}-lated by the subject invention) a nitrogen generator ofthe present invention would
have a lower production rate and/or produce nitrogen at a lower purity than a prior art
desigIL However, the present invention also c~ nt~nplates an operationa] embodiment in
which a c~,.,~ ,c,.l;on for such reduced reflux is effected by the provision of i,.~ .",~Ai~t~
25 reflux s~ns introduced into lower portions of lictill~tion column 30 where additional
liquid reflux is particularly nPedetl
The int~rmPdi~te reflux allows single column nitrogeD ge,le,8lor 10 to have the
sarne production rate of product and purity as could be cxpected in a similar prior art
30 plant design. To this end, second subsidiary stream 26 is liquefied within ~a?~l,ze. 54.
In order for there to be a t~ difference between oxygen emiched liquid st~earn

?159308
50, af'~er having been subcooled, and second subsidiary stream 26, pressure reduction
valve 55 is provided to reduce the plC~ and thereby the t~ pc,dtllre of oxygen
enriched liquid stream 50. This reduction in ple~ e of oxygen enriched liquid stream
50 is below the ~ ; of ~ tion column 30 and yet results in a sufficient ~Ics~l.e5 for oxygen cnriched liquid stream 50 that vapor stream 62, derived ther~olll, can serve
in a refrigeration role. At lower d~ tion column pless~lies, for ~ nre below 8
bar(a), additional reflux to ~i~tit~ on column 30 is produced by liquefaction of a vapor
stream 72 c~l,acled from lictill~tion column 30 at about the same point as second stream
26, after liquefaction, is intrc~uced into ~i~till~tion column 30. Vapor stream 72 is then
10 liquefied within vaporizer 54 and introduced as additional reflux above the point of
introduction of the liquefied second subsidiary stream 26. As is evident, I,~s~l,e
reduction valve 55 also serves to provide a ten~pe.atule difference between oxygen
enriched liquid stream 50 and vapor stream 72.
A possible variation to a~lus 10 involves operation of r~ tjon colllmn 30
at high p.essu~ In such case, an expansion m~rhine might also be ~t ~rh~i to coolant
stream 46. This would in~ l~ase total plant refrigeration and therefore the amount of liquid
produced. Additionally, such t~ A~.~nder could also be used to drive a recycle
COnl~ 5SOI to recycle part of the oxygen enriched liquid contained within coolant stream
20 46 back into distillation column 30 to also increase production. As can also be
appreciated, partial vaporization of oxygen enriched liquid stream 50 is not restricted to
the illustrated embodiment in which partial vaporization is effected through liquefaction
of a portion ofthe il~collling air. For i~ c~ in a proper low ples~ule colurnn
application, a stream from the col-~mll, not having the cxact composition of liquid air,
25 could be used in place of liquefied air.
With reference to Fig. 2, an altemative embodiment of single column nitrogen
generator 10 is illustrated. In nitrogen gencrator 10, oxygen rich strcam 50 after being
subcooled within su~cooler unit 52 is divided into first and second partial strea-m--s 50a
30 and 50b. First partial stream 50a is e~r~n-led in first pl~a~ule reduction valve 60 to form
coolant stream 46. Second partial strearn 50b afier having been e~cr~nded by pressure

2159308
reduction valve 55 is then fuily vaporized within vaporizer 54. The fiully va~l~ed
stream, design~ted by reference number 63, is then partially warrned within rnain heat
exch~nger 22 and exp~nded within turboexpander 64.
S EXAMPLE 1
The following is a charted, c~lull~t~d cxample of a possible operation of singlecolumn nitrogen gc.le.alor 10 (illustrated in Fig. 1) in accoldance with the present
invention. In such example it is ~csllrn~d that colurnn 30 uses low pl~s~ drop
10 s~ructured pflc~ing and has about 100 theoretical stages. Second partial stre~n 26 after
having been liquefied is added to the tlictill~tion column at about six theoretical stages
` from the bottom. Stream 72 is withdrawn from the dictill~tion column at a point of about
six theoretical stages from the bonom and returned after co~dl ncing to a point about
sixteen theoretical stages from the bottom of ~lictill~tioD colurnn 30.

2159308
CHART FOR EXAMPLE 1
Stream Flow Condition Tc~ ule P~esau~e~ 2 Content
No. Nm3/hr Liquid K bar (a) % or parts
Vapor per rnillion
12 13,400 V 305 1.01 20.96
24 11,739 V 93.0 3.17 20.96
26 1,454 V 93.0 3.17 20.96
47 3,901 V 87.6 1.21 53.32
S0 6,670 L 92.6 3.17 41.92
58 3,901 L 90.1 2.27 53.32
62 2,768 V 90.1 2.27 25.85
66 2,768 V 83.0 1.09 25.85
68 6,670 V 88.3 3.10 2 ppm
72 1,454 V 90.6 3.17 9.33
It is to be noted that in such example the letter "L" indicates a liquid condition
and the letter "V" indicates a vapor condition. Top product punty, nitrogen recovery as
fraction of the air feed, and addition and withdrawal points are sensitive to the physical
20 ~ro~, Lies of the data base employed in effec~ ;ng the c~lc~ tions. Losses inherent in
operation of the pre-purification unit have been included in stream 12. As would be
appreciated by those skilled in the art, subcooler 52 would be at a low elevation with
respect to the sump of ~ till~t;on column 30.
25Thus, in a prior art design making a gaseous nitrogen product, identical in quantity,
fractional recovery from air, purity and pressure, where a turboexpander makes
12

- ~159308
refrigeration by exr~nding air into the dictill~tion column, s~eam 12 would normally be
col~plcssed to about 3.94 bar(a). In the present invention, air co~ ,l.ssion will only be
to about 3.45 bar(a).
EXA~LE 2
Thc following is a cha~ed, calculated cxarnple of a possible operation of singlecolurnn nitrogen generator 10 (illus~ated in Fig. 2) in accordance with the present
invention. In such example it is ~sllme~ that column 30 uses low ~le;.~u~e drop
10 s~uctured pa~l~ing and has about 100 theoretical stages. Second partial strearn 26 after
having been liquefied is added to the ~ictill~tion column at about six theoretical stages
from the bottom. Stream 72 is withdrawn from the ~ictill~tion column at a point of about
six theoretical stages from the bottom and retumed af~er con.1~n~ine to a point about
sixteen theoretical stages from the bottom of tli~till~tion column 30.

2159308
CHART FOR EXAMPLE 2
Stre~n FlowCondition Te.. ~pc.atu~e P~saul~, 2 Content
No. Nm3~rLiquid K bar (a) % orparts
Vapor per million
12 13,400 V 305 1.01 20.96
24 11,259 V 92.6 3.10 20.96
26 2,080 V 92.6 3.10 20.96
47 3,889 V 86.3 1.21 41.92
6,669 L 92.4 3.10 41.92
50a 3,889 L 87.0 3.03 41.92
63 2,780 V 92.1 2.18 41.92
66 2,780 V 85.2 1.06 41.92
68 6,670 V 88.0 3.03 4.8 ppm
72 1,008 V 90.3 3.09 9.06
While the present invention has been tescribed with .cife.e,~cc to a ~lcf~.led
embodiment, it will be understood by those skilled in the art that numerous changes,
20 additions, and omissions may be made without departing from he spirit and scope of the
present invention.

Representative Drawing
A single figure which represents the drawing illustrating the invention.
Administrative Status

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Event History

Description Date
Time Limit for Reversal Expired 1999-09-27
Application Not Reinstated by Deadline 1999-09-27
Deemed Abandoned - Conditions for Grant Determined Not Compliant 1998-10-06
Deemed Abandoned - Failure to Respond to Maintenance Fee Notice 1998-09-28
Notice of Allowance is Issued 1998-04-06
Letter Sent 1998-04-06
Notice of Allowance is Issued 1998-04-06
Inactive: Status info is complete as of Log entry date 1998-03-24
Inactive: Application prosecuted on TS as of Log entry date 1998-03-24
Inactive: IPC assigned 1998-02-20
Inactive: IPC removed 1998-02-20
Inactive: First IPC assigned 1998-02-20
Inactive: Approved for allowance (AFA) 1998-02-20
Application Published (Open to Public Inspection) 1996-04-26
Request for Examination Requirements Determined Compliant 1995-09-27
All Requirements for Examination Determined Compliant 1995-09-27

Abandonment History

Abandonment Date Reason Reinstatement Date
1998-10-06
1998-09-28

Maintenance Fee

The last payment was received on 1997-09-11

Note : If the full payment has not been received on or before the date indicated, a further fee may be required which may be one of the following

  • the reinstatement fee;
  • the late payment fee; or
  • additional fee to reverse deemed expiry.

Please refer to the CIPO Patent Fees web page to see all current fee amounts.

Fee History

Fee Type Anniversary Year Due Date Paid Date
MF (application, 2nd anniv.) - standard 02 1997-09-29 1997-09-11
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
THE BOC GROUP, INC.
Past Owners on Record
ROBERT A. MOSTELLO
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
Documents

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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Abstract 1996-04-26 1 21
Description 1996-04-26 14 612
Cover Page 1996-06-18 1 18
Claims 1996-04-26 10 327
Drawings 1996-04-26 2 39
Representative drawing 1998-02-04 1 18
Commissioner's Notice - Application Found Allowable 1998-04-06 1 165
Courtesy - Abandonment Letter (Maintenance Fee) 1998-10-26 1 184
Courtesy - Abandonment Letter (NOA) 1998-12-29 1 170
Prosecution correspondence 1998-02-19 1 32
Prosecution correspondence 1995-09-27 1 25
Prosecution correspondence 1995-11-07 2 26