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GB329427A.pdf

GB329427A.pdf

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Herculos company patents
Herculos company patents

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,-
PATENT SPECIFICATION
Oonyention
Date
(United
Sta.too):
Jan.
28.
7929.
329,427,
Application
Date
(in
United
Kingdom):
Maroh
9,
7929.
No.
7781/29.
Complete
Acceptld:
May
22,7980.
COMPLETE
SPECIFICA~ION.
Improvem.ell·~
in
Me'&hodof
Producing Nitric Acid.
We,
HERCULES
POWDER
COMPANY,
acorporation ,organized under the laws
or
the State
of
Delaware,
one
of
the UnitedStates
of
America,
of
900,
Market Street,
ti
City of Wilmington, State
of
Delawlare,United States
of
America, Manufacturers,Assignees of. J
AMES
HERBERT
SIIAPLElGH,
a citizen
of
the United States
or
America,
of
Mountain
I.Jakes,
County
or
Morns,
10
State
of
New
Jersey, United States ofAmerica,
do
hereby declare the nature
of
this invention and
in
what manner thesame
is
to
be
performed,
to
be particu
larly
described and ascertained in and by
15
the following
statement:-
This inv'ention relates
to
an improve
M
ment in method
of
producing nitric acid
,and
more particularly
to
a novel methodinvolving the absorption
of
oxides
of
20
nitrogen
land
has for its object to providea method and apparatus whereby nitricacid may
be
produced
by.
absorption
of
nitric oxides in a highly
effiCient
manner,with the production
of
an acid of high
21).
concentration and without substantialcapital outlay or substantial operatingcost.
In
aacordancelwith this inveniiiou,there is provided a single
one
pass tower
30
of
suitable dimensions and suitablypacked
so
that
starting-with water thenitrogen oxide gases will be subJected toabsorption by nitric acid
of
constantlyincreasing concentration contacted in
3lS
counterflow with the gases in constantlydecreasing concentrations, under conditions approximating conditions
or
equilibrium. .. Heretofore
it
has
,been
knc)'w:u
to pro-
!~Cl
duce nitric acid by ,absorption
of
nitrogenoxides, and
the
method generally used,and known. as the multiple. tower method,involves the passing of the
o:scides
in
gaseous form through a series
of
packed
45
towers thliough
which:
nit:rie acid is
ci1'
, culated and
ab'sorbs
the o±ides.
With
theuse
or
a series
or
towers, the oxides arepassed through the series' in
cOllllterfloW'
with
nitric
acid$
the first tower
1'ec'eiving
no
the richest oxide vapors and the strongestacid while'
the
last t6wer
1!eeeives
theleanest-
V'apors
an([
~entain8'
the weakestacid, water being added
to
the last tower.
[P'I'ioe
1/~]
The nitric acid in each tower
is
of
substantially definite strength and a
lal.'ge
[};)
quantity
or
acid is
cir?ulate~
thro:ugheach
of
the towers, the
CIrculatIOn
bemg,for ex.ample,
at
the rate of
£rom five
totwenty gallons per minute, the towers beingpacked,
ro1'
example, with quartz or
some
t$()
form
of
chemical
war'e
ring.Another method in general use and
Imown
as
the common plate columnmethod, involves pooling
of
the absorb-ing acid and absorption is effected, with-
61'}.
out circuLation of the acid, by bubblingthe oxides through the absorbing acid.The multiple tower system
is
relati:velyinefficient due
to
the fact
that in
each
of
the towers equilibrium between the gases,
70,
which enter the several towers
at
a
de£.-
nite concentration, and the absorbingacid, which also enters the several towers
at
la
definite concentration,
is
quicklyapproached and absorption practically
7G
ceases before the gases have travelled anyappreciable distance
in
a.
tower in con-tact with the
lacid,
with the result
that
a limited quantity of absorption takesplace in each tower,
at
a given
ten1pera~
8G
tur~,
which results in great waste
of
towerspace and excessive capital investmentin towers and packing thtlrefor. Thiscondition
of
equilibrium . can only bechanged by a relative difference
in
the
8IS
Doncentmtion
of
the gases relative to theconcentration of
thEl'
absorbing acid;
as
by
the oxidation
of
NO
to
N0
2;
whichrequires
ti.me.
Thus, to obtain desiredconcentration with multiple towers
it
is
90
necessary
tD-
have
ia,
large tower volume;in order
to
bring about changes in relative oxide c6ncentrations for contact withthe strength
of
acid being circulated.
It
is
furth~r
rtecessf£ry
to
cirenl~te
a large •quantity
of
.
:toid
through the severaltowers,
to
minimize change in
con~entra-
tioI):
and temperature, and to pass the
a:cid
and oxides
fr{)m,to:we:r'
to
tower,;
dbtaining
par~ial.
absorpti.on
ip.
the
.
sev'erall
towers
100
respectlvely
untJ;l
subst:;tntHtltota~
absot£)'hiD-nis
obtained. The
m;q:ltiple
towElr
me'thod is substantially inefficient due
to
ineffieieiit absorption
in
,the! resnective
toWel.'S
due to
the-
rf1pidity with which
a;
IOl{
condition of equilibrium
is
approached
 
2
329,427
and
to
the
consequent requirement for asubstantial number of towers, aggregat
ing
a large length of pass
and
large tower
-yolume,
and
to
the
necessity
for.
fuech-5 anically
lifting
large quantities ofabsorbing acid from
the
Qottom' of a preceding tower to
the
top of a succeedingtower to effect
the
circulati<m thereofthrough
the
system
whereby he
gases
and
have smooth continuity of reaction
buthasthe
opposite,
rapidly
changing inter
mittent
sequences of reaction.
In
carrying this invention into prac-10 acid may enter
the
several towers
in
relative concentrations such
that
a conditionof equilibrium will not exist
in
the
several towers on
their
entry.The multiple tower system is :further
i5
inefficient, due to
the
necessity
o:f
usingrelatively inefficient tower packing
in
order to allow circulation of
the
requiredamount of acid and. to
the
fact
that
largetower vohtme excludes efficient
heat
20
e;s::traction,
with
the
result
that
the
large
quantity
of acid circulated for minimiz
ing
the
t.empera~ure
rise must
'deJ>~nd
upon coolrng entll'ely
apart
:from
the
tower itSelf.·
In
practice, acid coolers are
25
:provided involving considerable capitalexpense.The common
plate
column method isalso substantially inefficient due to
the
fact
that
in
bubbling the oxide gas30
through
the
pools of absorbing acid lackof vigorous diffusion set
up within
the
bubbles and
at
the
interior surface thereof,where there exists a
m{)re
or less dead
layer
of exhausted gas
and
a layer of con-,
35
centrated acid,
and
local
high
temperatures
iat
the
bubble walls create difficulties which render absorption
highly
inefficient.
In·
connection
with,
the
common
plate
column,
it
will also be40 noted
that
there
is
an
absence
{)f
multipleincrements of
varying
acid strength,
the
benefit· of a discontinuous
rather than
acontinuous film, etc.The common
plate
column method
is
. 45 essentially one dealing
with bulk
acid
and
involving discontinuous absorption,
and
comprises what
might
be termed a seriesof
rapid
absorptions far removed fromconditions of equilibrium ancl separated,50
by
oxidation steps wherein
NO
is oxidized
to
magnitudes
by the
order of
80-90%.
As practised, p1ate
columri.
systems aregenerally under presf.lures of
6-8
atnlospheres
at
the
present time, and utilize(55 gases entering animpnia
,oxidation'
con
verters
of about 8-:-9%
NRJl
content-byvolume. _ '
It
is evident
that
th~
plate
cQl:umn·
is
not
dealing .
with
thin
fihr.ls
of acid w:hich,60 constantly challge
hut
rather with
bulkacid of appreciable.
imensio~s.
The.
platecoliilll.1lattempts to. function on a
large
scale
basis,trymgfor-
bulk
abso.rptioll,
perplate~,
bulk
o#dation
-per
·chamber,
:65'
andbulkextr~;ctioI).
ot~eat.
It
dQe.s.-ndt
tice, nitrogen oxide gases are passed ill
70·
counterflow
with an
absorbing medium,
as
nitric
acid, under conditions :approxi
mating
equilibrium conditions, the acid
and
gases flowing oppositely
in
a singlevertical pass
in thin
films, desirably
or
750
rapproaching unimolecular thickness, theacid being divided into
an
indefiniteh'large number of increment acid strengths,
:fixed
by the
work of absorption
and
,blending one into another
so
that
the
80'
acid strength gradient is a smooth one.
At the
same time
the
oxide gas is dividedinto
an
indefinite large number or increments of different concentrations blend-
ing
into one another, thus both
the
lacid
85.
strength gradient and
that
or
the
gas issmooth.
In
oarrying this invention
intopractice; the
nitrogen oxide gases, desir
ably'
substantially free from diluent
-gases,
though
it
will be appreciated
that
9()
my
method is adaptable to
the
treatmentof nitrogen oxides obtained from mixtures such as 'nitric and sulphuric acid
,as
used
in
recovering
and
concentrationoperations, are admitted
at
the
bottom of
95-
a vertically extending tower, preferablyof substantial height
as
compared with itsdiameter,
intothe
top of which water isadmitted. The tower is
so
packed as togive
an
adequate
fi.hr.t
surface, large free
WO<
space
and
short vertical movement, while
at
the
same time
it
is adequately cooled,for example,
by
water
or
refrigeration,
so
as
to effect removal of
the
heat of reaction
su~stantially
simultaneously
with
its
:1.05
generation. The free space, while pur--posely made ·extra large, is also purposelysplit
up
into small chambers.
It
is
in
these chambers
that
oxidation of
NO
to
N0
2
takes place,
the
oxygen for the HI)reaction being supplied
by air
introduced into
the
tower either independentlyor together with the nitrogen oxide gases,and due to
the
limited
unit
size, oxidationoccurs only to a small extent therein.
ii5
The oxidation
.as
a whole takes place
through
the
arge
free space provided when
all
of
the
small chambers are _considered
in
aggregate. The
.c1ra::nrbers~
so
provided
by
splittiIlg
_up-
-the free space into an
f2()
unusually large number of small units is .essential
to the
functioning of the towel'
so
close to its equilibrium conditions,
and
hence
tothe
advantages obtained.The
water
-entering
the
top or
the
tower,
125
in
.quantity sufficient
fm the
concentration desired, absorbs upwardly flowingoxides rorming dilute nitric acid,
and
flow:ing
.downwa,rdly through the tower
at
a
relatively slow
rate
.under control of the
130
 
329,427'
3
packing therein continues to absorboxides becoming constantly more concentrated.
As
its downward
flow
progresses,absorption is facilitated by the adequate5 film surface and adequate free space, andby the fact
that
the oxide
gtases
in theirupward passage through the tower arecontacted with the absorbing medium
at
ever decreasing concentrations
of
oxides
iO
and by the fact
that
while
as
the
NO
of
the upwardly flowing gases oxidizes to
N0
2,
it
is
contacted with acid
of
nearlythe exact strength to estuMish a
con
dition of equilibrium
at
the point
of
con-
i5
tact, while in the counterflow of acid andgases the
NO,
is
immediately afterwardcontacted with acid
of
a slightly weakerstrength which promotes absorption and
so
on
throughout the tower, with the
20
result
that
the oxidation
,and
absorptioncontinu.es from the bottom
to
the top otthe tower smoothly and without the existence
of
a single state
of
equilibrium for
any
appreciable distance up the tower and,
25
w,ith
discharge
fro~
the tower
of
. hIghly concentrated
aCId,
The practical adaptation
of
the methodembodying this invention will,
it
is
believed,
be
understood
in
connection
30
with the following description
of
la
preferred embodiment
of
a form
of
apparatus embodying. my invention,
as
illustrated in the accompanying drawings,and adapted for use in the practice
of
the
35
method, the practice
of
which, however,
it
will
be
understood, is not dependentupon the use
of
any particuLar form
of
apparatus,
In
the drawings:
40
Fig,
1
is a diagrammatic view
of
atower embodying this invention, partlybroken away to disclose the packing,Fig. 2 is a detail view, in perspectiveand partly broken away, of a form
of45
packing for the tower shown in Fig.
1.
.
In
the drawings
a
indicates a vertically·extending tower, which may
be
made
of
chrome iron and may conveniently be,say,
thirty
to forty feet in height and
of
50
a diameter of, say, from eight to fourteen inches, though
it
will
be
understood
that
the exact
size
of
the tower withinrelatively wide limits is unimportant,
it
being only necessary
that
the towel' be
55
provided with means for adequately, removing the heat
of
reaction, or
that
it
be
of
a diameter such
that
the coolingmeans _herein' described may effectivelyremove the heat. At the top of the tower
60
is provided a pipe
b
through which the, spent gases pass from the tower, while
at
the bottom
of
the tower a pipe
(J
is
P1'O
videdthrough
which the nitric
oxid-e
gases to be absorbed are admitted
to
the
~6_5
tower. A pipe
d.,
connected to a. water
slLpply,
extends into the top
of
the towerand is provided.
on
its
·end
within thetower with
.a
spray head
e.
The pipe
d
is
provided with a suitable valve
f
forcontrol
of
the supply
of
water
to
the
70
tower.Adjacent
to
the top and bottom
of
thetower
a,
and also intermediate betweenthe top and bottom,
,are
positioned flanges
g,
g1
and
gll.
The
flanges.
g
and
gl
are 75arranged
so
as
to
_provide
annular openings
h
about the
out!:)r
surface
of
thetower, while the flange
gn
is
closedwith the wall
of
the tower. A pipe
i
provided with a valve
j
,affords
a supply of 80
w,ater
to
the flange
g
and a pipe
le
drainsthe
flang'e
gll
which receives waterflowwing
down
the outer surface 'of the towerfrom flange
{J
to
and through flange
gl,
A pipe
0
serves for withdrawing the
con-
85centrated acid from the bottom
of
thetower
a.
The tower
a
is
packed with a suitablepacking, which may, for
eXlample,
be
as
is illustrated in detail in fig.
2,
compris-90ing a plurality of glass cylinders
m
superimposed on
one
another and withineach
of
which is
,an
insert,
as
£.01'
example,an irregular lump of quartz
11, 01'
ofchemical ware,
of
a size substantially less 95than the interior area
of
the cylinders.The packing
is
of
a type having high surface value and large free space. Thepacking is made
of
a breadth and height
;and
has a center piece such
that
for a
100
given
flow
of liquid a given
flow
of gasproduces conditions
of
turbulence favorable to both heat transfer and absorption.By way
of
illustration,
in
carrying outthe method according
to
this invention
105
with use of the apparatus described .above, . nitrogen oxide gas, desirablythrough not essentially substantially freefrom diluent gases,
is
admitted
to
tower
a
through pipe
c
from
any suitable source,
HO
Water is admitted to the top
of
the
t-ower
in the form of a spray from pipe
d
and
w,ater,
is admitted
to
the flange
g
throughpIpe
~.
The nitric oxide gases rise in the tower
H~
through the packing, which retards theirprogress and causes them
to
travel horizontally in travelling generally
in
asingle vertical direction upward throughthe tower, The. gases are also
cal1sed
to
120,
spread out in films
on
the packing -",elements. The water entering the tower
flows
downwardly
inthe
tower
in
connter
flow
to the rising
O',ases
and its
flow
isretarded by the packing and
it
is caused
125-
to
flow
horizontally
in
flowing generally .vertically and is spread out
in
films
on
the packing'. . The upward flowing gasescontact with the downward flowing wateradj.acent to the -top of the tower and
13();

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