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GB333264A.pdf

GB333264A.pdf

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Herculos company patents
Herculos company patents

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PATENT SPECIFICATION
Convention
Date
(United
States)
:
Oct.
26,
1928.
333,264
Application
Date
Un
United Kingdom):
Feb.
6,
7929.
No.
8906/29.
Oom
p/ete
Accepted:
A
ug.
6,
7980.
COMPLETE SPECIFICATION.
Improvements
in
Methpd
and
Apparatus
for
Denitrating
Mixtures
of
Nitric
Acid
and
Sulpp.uric.
Acid
and
Ooncen-
trating Nitric Acid.
"Ve,
HERCULES POWDER
COMPANY,
a corporation organized under
the
laws of
theState
of Delaware, one of
the United
5 States of AmeriNl., of
900,
Market Street,City of
Wilmington, State
of Delaware,
lTl1itec1.
States
of
America, Assignees of
JAMBS
LEROY
BENNETT,
a citizen of
the
t'"nited States of America, of
Wilming-
10
ton, County of New Castle, State of Delaware,
United
States of America,
do
hereby declal'e the
nature
of this invention
aUll
in
what
manner
the
same is to beperformed, to be
particularly
describedand ascertained
in
and
bv the
following
15
statement:-
This invention relates to a method
and
(l,ppuratus for
denitrating
acid mixtures
and.
more
particularly
for effecting
the
concentration of
nitric
acid.
"~20
The object of this invention is to
pro~
vide a method
and
appar.atus adapted forthe denitratiDn of acid mixtures) or
the
concentration of
nitric
acid of such
char~
_ acter
,as
to avoid
the
necessity for
any
sub~
20
stantial
excess of dehydl'ating agent, .andwhereby not only is the process renderedmore economlcd
but
the
obtaining of
the
desired concentrated
nitric
acid is assured.Accerdingly, the present invention com-
30
prises
the
method of concentrating
nitric
add
which includes passing a
mixture
ofaqueous
nitrie
acid
and
a:
dehydrator
in
countel'flow
with
a
mixtU1'e
of
steam andnitric
acid vapour to effect
partial
deni-
35
tration
of
the
former mixhlre,
heatingthepartially
denitrated
mixture
to generatesteam
and nitric
,acid vapour
and
utilising
a-
portion of
the
generated steam forthe clenitration of
further
quantities of
40
the acid
mixture, and
effecting
the
separa
tion
or nitric
lachI
from
the
balance of
the
steam generated,
the quantity
OT
steam
passing
into
the
tower
in
which
the
counterflow takes place being limited to
45
an
extent
necessary for a'Voiding excessivedilution of
the
concentratecl
nitric
acicl.
As
the dehydrator,
sulphuric
acid,phosphoric acid, anhydrous sodium sulphate
or
any
other suita-ble
material may
50
be used.
In
the
practical ,adaptation ofthis inYentioll,
the partially
denitrated
[Price
1/"] -"
acid
mixture
is
so
accumulated
and
boiled
as
to apportion to contact
withthe
mix
hue
to be denitr.ated only such
quantity
of vapours
as
will
contain such
water
55vapour as is necessary to drive
off
thenitric
acid from
the mixture,
while
at
the
same
time
effecting
the
recovery or
nitric
acid from
the
balance of
the
vapoursboiled
off
from
the
accumulation.
60
Referring
now to
the
accompanyingdrawing,
in
which
an apparatus
embody~
ing
this invention is
illustrated
diagrammatically,
and
in
connection with adescription thereof
the
practical adapta-65tion or
the
method will be described,
a
indicates a 'container ror a
mixture
of,acids which
may
be composed, rorexample, of
30%
HN0
3,
50%
H
2
S01
and
70
20%
H
2
0.
The container
a
is connected
by
a
pipe
b
with
a tower c, packed
with
a suitableacid proof !lacking
d
supported
by
a suitable perforated support
e.
Beneath
the
tower
c
rand
connected thereto
by
a pipe
t
75is
.a
vessel
(J
formed from acid proof
material
and
prov.ided
with
hollow walls
h
into which steam
maybe
fed from a suitable source
through
a
pipe
i
for
the pur
pose or
heating the
vessel. The vessel
g
80
is divided into three compartments
j,
jl
and
jll
bv
means of j)artitions
le
spacedfrom
the
·bottom of
the
vessel
to permitthe
passage of
liquid
but
not
of vapourfrom
on'e
compartment to another.
Each
85
of
the
compartments
j,
j1
and
jll
containsa steam
coill
receiving steam from pipe i,which is also connected to
the
interior of
the
hollow walls or vessel
(J,
while a pipe
90
me,
providerl
with
a steam
trap
rnl,
servesfor disch.arge of steam from
the
coils
and
from
the
walls of vessel
g.
The
pipe
f
affords communicationbetween
the
tower c
and
cDmp,artment
j
of vessel
g,
while compartments
j1
and
pI
95are connected
withthe
tower
71·
by
a pipe
0,
connected
to the
tower
at
a
point
aboveits bottom
and
a
branch
p
therefrom,respeeti:vely. A
pipe
2,-
provided
with
abend f-orming a tr.ap 3, is connected
at
100
one end to
the
tower
n
at
its
bottom,while its other 'end extends into chamber
 
2
333,264
i.
The tower
n
is packed
with
acidresisting material
q,
supported on a perforated acid proof plate
T.
'fhe
vessel
g
is provided with
an
overflow pipe
gl
to5 maintain a level
in
the
vessel well
labove
the
lower edges of partitions
k.
The top of tower
n
is connected
to
,a
reflux condenser
8
packed with a suitableacid resistant packing
t
and
provided
at
10
its topwitli-an outlet
t.
The top of tower
c
is connected to a c.ondenser comprising acoil
'v
within a casing
w
into which cool
ing
water is introduced through a pipe
x,
an
overflow pipe
'Y
being provided to
15
maintain a leveL' The coil
'D,
at
its lowpoint, is connected by a suitable pipeto
a
receiver
z
adapted to receive condensed nitric acid,
ancI
the
end of
the
coildischarges into
an
absorption tower, not
20
shown, wherein
any
lower oxides ofnitrogen resulting from unavoidabledecomposition of nitric acid are absorbed.
In
the
.
earrying out
of
the
method
in·
accordance
with
this invention a mixture
25
of acids, for example, comprising
30%
HN0
3,
50%
H
2
S0
4
and
20%
H
2
0,
is provided· in container
a,
land a mixture ofsulphuric
add
and water,
say
60-65%
H
2
SO"
in
quantity to
fill
the
v-essel
up
30
to
the
o,erflow pipe
gI,
is provided
in
thevessel
g.
The vessel
g
is heated,
bythe
admission of steam
to
coils
l
and to the
interior of
the
walls of
the
vessel
to
boil
off
water vapour from
themixture
35
therein. The vapouril boiled
off
in the
compartment
j
pass through pipe
f
land
:flow
upwardly
in
tower
c
in~o:unter
:flow
to
the
downward
:flow
of
the
mixture ofacids from container
a,
while
the
vapours
40
from compartments
j1
and
jII.
passthrough pipe
0
and
branch
p
into tower
n.
The downftowing mixture of acids
in
tower
c
is denitrated
by the
water vapourfrom ehainber
j
and.
the
nitric acid
45
vapours pass from
.the
tower into coil
'I)
wherein thev are condensed and fromwhich
the
concentrated nitric acid passes
to
receiver
z.
The denitrated. or
partly
denitrated ,acid mixture
flows
from
the
50
bottom of tower
c
into chamber
j
of vessel
g
through pipe
f
and
the
:flow
of
vapoursfrom chamber
i
through pipe
2
is prevented
by the trap
3,
which is full ofliquid, as will be described. The original
ti5
sulphuric acid
and
water
in
vessel
[J
isdisplaced
by
the partly
4enitrated mixture, from tower
c,
whIch may, forexample, . comprise say about
55%-65:%
R,S04
and say about 1
%-3%'
HNO
a,
and
60
whic11
is boiled
in
. vessel
{l
prodilcingvapours of water
and
of such nitric acidas was not removed from
the
acid mixture
in
tower
c..
The nitric acid vapours produced
in
vessel
g
and
passing to tower
e
65
through
pipe
f
will
p.ass
Iromthe
tower cto
the
condenser with
the
nitric acidremoved from the acid mixture fed intothe tower.As
has
been indicated, the vessel
g
isdivided into compartments
:!'rom
only one
70
of which water vapour passes
to the
tower
c
and
such compartment is
so
proportioned
that
.<mly
such
amOlmt
of water vapourwill pass from
the
vessel
g
to tower
c
asis necesSary for denitration of the
aeic1
75
mixture
in·
the tower,
or
in
{lther words,the passage
'of
an excess of water Tapourto tower
c,
which would result
in
dilutionof
the
separated nitric acid, is avoided,
as
is also any substantial excess of dehy-
80
drator,
the
latter
being achieved
by
sup
plying
to the tower only substantially theamount of dehydrator required.The ,acid mixture in its passage throughtower
c
is not completely denitrated and
85
it
will
be
noted
that
such nitric acid
as
passes into vessel
g
will
be recoveredeither
by return in
vapour form fromchamber
i
to
t{lwer
c,
with subsequentpassage to the condenser with separmted
90
nitric .acid, or
by
passage with watervapour from chambers
p
and
pI
throughpipe
0
and
branch
p
into tower
n
and thereflux condenser
s
in
which
the
nitric acidwill be condensecl, to
flow
back from the
95
bottom or tower
li
to chamber
j
of
vessel
g,
through pipe
2,
for vaporization and,eventual passage into tower
c,
and fromwhich
the
water vapour will be dischargedthrough
outleitl.
The nitric ,acid flowing
WO
from tower
n
to
compartment
j
thmugh
pipe
2
fills
the
trap
3
and,
as
has beenindicated, prevents
the
:flow
of vapoursfrom chamber
j
through pipe
2.
In
connection with
the
abov-e
descrip-
105
tion of this invention,
it.
will be understood
that
the
nitric and sulphuric
:acid
may
be
introduced into tower
c
as
a mixture, or separately
if
desired
,ancl
that
theyessel
,q,
or its equivalent, may be divided
110
mto two or more compartments
as
com
pared to three compartments
as
described,or the. requisite lamolmt of water vap01ll
maybe
supplied to
the
tower
(J
in
anyother manner from the
partially
deni-
i
hated
mixture.
i
5
Having
now particularly described andascertained
the nature
of our said invention and
in
what manner
the
same
is
to
~)e
p.el'formed,
we
declare
that
what
we
120
claIm
1S:-
L The method of concentrating nitric;acid which inchtdes passing a mixtureof aqueous. nitric acid and a dehydrator
in
counterflow with a mixture of steam
125
and.
nit~ic
acid vapour to
~:ffect
partial
dellltratlOn of
the
former mIxture heat.
ing
.
he partially
denitrated
mixt~re
to
generate steam and nitric acid vapour .andutilising a portion of
the
generated steam
130
 
333,264
3
for the denitration of further quantities
of
the acid mixture, and effecting theseparation
of
nitric acid from the balance
of
the steam generated, the quantity
of
5
steam passing into the tower in which thecounterfiow takes place being limited
to
an
extent neeessary for avoiding excessivedilution
of
the concentrated nitric acid.
2.
The method
of
concentrating nitric
10
acid substantially
as
described herein.
:3.
Apparatus for the concentration
of
nitric acid including a tower for
contact~
ing in counterfiow aqueous nitric acid
and
la
dehydrator with steam, a vessel for
15
the collection
ofacicl
mixture from the, tower, means
for
dividing said vessel intocompartments connecting
at
a point belowthe normal level
of
the mixture in saidvessel, means
101'
generating steam ,andnitric acid vapour from the mixture in
20
said vessel, and
la
conduit for the passage
of
steam and nitric acid vapour
to
said
towel'
from
one
of
said compartments only.
4.
Apparatus in accordance with claim
3;
characterised by the fact
that
means
25
101'
separating nitric acid from. steam areprovided
in
communication with another
of
said compartments.
5.
Apparatus for concentrating nitricacid substanti,ally
as
illustrated and
30
described herein.Dated this 5th day
of
February,
1929.
HASELTINE, LAKE
&
00.,
28,
Southampton Buildings, London,England, and
19-25,
West 44th Street, New York,U.S.A.,Agents for the Applicants.
Redhill: Pdntf'rl for His Majesty's Stationery
Office,
by Love
&
Malcomson,
Ltd.-1930,

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