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Патент USA US2127360

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Aug. 16, 1938.
J. HELLE ET AL .
2,127,360
'_ PROCESS FOR THE REMOVAL OF ACID FROMYNI'I‘RATED STARCHx
Filed Nov. 10, 1956
4 Sheats-Sheet_ 1
A TrMM/EY
Aug. 16, 1938.
J. HELLE ET AL
2,127,360
PRQCESS FOR THE REMOVAL: OF ACID FROM NITRATED. STARCH
' Filed NOV. 10, 1936
4 Sheets-Sheet 2
‘Aug. 16, 1938.
J. HE'LLE Er AL
2,127,360
PROCESS FOR THE REMOVAL OF ACID FRQMNITRATED STARCH
Filed Nov. 10, 1936
4 Sheets-Sheet 3
2»
‘v11 .
2g4"“; 1%
BYW ‘ a? 9mm
ATTORNE Y
‘Aug. 16, 1938.
* J.~HELLEETAL
2,121,360
PROCESS FOR THE REMOVAL OF ACID FROM NITRATED STARCH
' Filed Nov. 10, 1936
4 sheetsé-sheet 4
MM
v Fly
Wk“?
Wz2w
ATTb/VNE)’
Patented Aug. 16, 1938
. 2,127,360
, '
UNITED ‘STATES PATENT OFFICE
'
2,127,360
PROCESS FOR THE REMOVAL OF ACID FROM
/
'
NITRATED STARCH
Johann Belle and Alfons Kunz, Fuzfo, Hungary,
assignors to Nitrokemia Ipartelepek Reszveny
tarsasag, Budapest, Hungary
Application November 10, 1936, Serial No. 110,187
In Hungary May 22, 1936
3 Claims.
(or 260-148) _
This invention relates to a process for the re
moval of acid from nitrated starch. '
The invention provides means for a continuous
operation in a particularly economic manner, so
5 that the acid removed from the mass can be used
again in further operations.
_
'
Fig. 1 is a plan showing particularly the driv
ing means.
‘
'
It is known to remove the free mixed acid from
nitrated starch by covering a layer of the ni
trated starch of approximately uniform thick
w. mess with a mineral acid of the same speci?c
gravity, and in the same amount as the mixed
Fig. 1a. is a plan view of a portion of Fig. 1.
Fig. 2 is a detail of Fig. 1.
Fig. 4 is a. plan of the attachment.
Fig. 5 shows on an enlarged scale the puri?
cation arrangement of the attachment.
Fig. 6' shows a section on the line Vii-VI of 10
Fig. 5.
in again as concentrated acid. Themineral acid,
for example sulphuric acid, contained in the mass
after displacement of the mixed acid is then re
placed ‘by water, and thereupon the mass is
washed. This procedure isdi?icult to carry out
ti) in a, continuous operation, and uses up a con
siderable amount of acid.
‘
>
_
The invention provides a process for overcom
ing the above ‘mentioned dimculties, and the
nitrated starch is arranged in separate batches
es in a series, and these batches are treated in couns
tercurrent with water and freed from the mixed
‘acid. The separate masses of nitrated starch
‘identical one with the other are spread in layers
.
7 shows a section on the line VII-XII of
acid contained in the mass, and thereby displac
ing the mixed acid in the mass. The displaced
mixed acid is freed from water and can'be used
'
Fig. 3 is a longitudinal section on the line 5
III-III of Fig. 1.
Fig.
.
Fig. 8 shows the acid ‘delivery to the separate
cells.
'
Fig. 9 shows the arrangement for conducting
the, nitrated starch to the attachment.
'
Corresponding parts in‘the drawings are indi
cated by similar reference numerals.
,
The perpendicularly disposed shaft Iii is driv- w
en ‘by the shaft it by means of the bevel sear
ing it and it. The shaft it rotates intermit
tently and is operated in this manner by the elec
tric motor it through the co-roperating drive
shown in Fig. 1. The motor it drives the shaft 25
it by means of the spindle it and worm gear
H.
An eccentric it is keyed on to the shaft
llll and supports therod ii by means oi‘ the
of the same thickness on ?lter stones arranged ‘ roller 2%. The rod ii is rotatably mounted on
cc- separately one from the other in a common car _ the pivot 22 and is loaded with the weight it so
at its free end.
rier, and washed out with water in such a man
The rod ti carriesv a co-operating pawl tilt
ner that the pure water is conducted to the mass
already repeatedly extractedand containing the which engages in the teeth of the cog ‘it and
turns the shaft 112 through an angular distance
least amount of mixed acid and the acidi?ed wa
ter obtained at this point is successively con
ducted to nitro starch masses containing more
and more mixed acid. The aqueous acid drawn.
from the last mass ‘of the series is removed and
can be used as concentrated acid, for example,
40 in nitrating fresh starch. If the nitro starch
from which the acid has been extracted is re
moved for further operations and replaced by
a corresponding amountof crude nitrated starch,
the removal of acid can proceed without inter
45 ruption of the operation but before replacing the
washed out nitro starch with a fresh batch of
acid-containing nitro starch the ?lter stone on
which the latter is to be placed must ?rst be
freed from water, for example, in the manner as
[,0 hereinafter to be described.
'
equal to the pitch of the said teeth with each 35.
rotation of the eccentric.
At the upper end of the shaft ii an attach
ment ill is ?rmly keyed thereto so that this part
ll moves with the shaft ii.
The attachment
made, for example of acid resisting steel carries so
on its upper surface a series of segment shaped
openings arranged in a circle one beside the other
into which openings ?lter stones idi—dbd are
?tted to make a close ?t. Under the ?lter stones
28l—3i|3 hollow spaces 29 are provided in the in- 45
terior of the attachment each of which hollow ‘
spaces open into a channel 3d also in the inte
riorv of the attachment. The lower openings M
of all these channels lie on a horizontally ar
ranged annular sliding surface 32 of the attach; 50
ment on which the attachment slides on an edge
The apparatus in accordance withthis inven
tion is constructed for continuous operation. _ 33 also forming a sliding. surface of a circular
The invention will now be further explained by shaped member 35. Slots 342-350 are out along
reference to the accompanying drawings in the entire sliding, surface 35 which slots are of
different lengths for a purpose which will be here- 55
55Xwhich:—
2
inafter made clear. Each of these slots Ill-450
open into ?exible tubes til-3" through vwhich
the contents of the channel It and the hollow
spaces 2! may be conducted away. The'circular
cam disc ‘I4 arranged on the hollowshaft ‘It. The
hollow shaft 18 coaxial with the shaft I! is driven
by the shaft is of the worm drive l1 and the
chain ‘It and chain wheels ‘II and ‘l1.
'member 35 is ?rmly pressed against the sliding
7 _These transmissions are so selected. that the 5
‘ surface 02 of the attachment by means of a num
hollow shaft 1; and the cam disc ‘I4 arranged
her of springs 31 so that the wearing of the slid
ing surfaces can cause no leakage between the
contacting surfaces.
The lower ends of the
10 springs 31 abut on the fixed housing 38 of the
shaft
ll.
‘
_
A frame 39 having four pyramidal sides lies
on each of the ?lter stones Ill-403. This pyra
midal form serves the purpose of preventing the
15 ?lter cake being carried up with the frame when
the latter is raised.
Each frame 39 is attached to an arm 40, all
the arms 40 turning ona ring of pivots ll. A
ring 42 is ?xed on the attachment between the
frames 89 and the pivots ‘I, and the upper edge
43 of the ring is slanted outwardly and provided
thereon together ‘with abutment ‘II makes one
revolution whilst the pawl 25 turns the shafts l2
and I I through a part of a rotation corresponding
10
to the pitch of the teeth.
The number of teeth of the wheel I! is the same
as the number of ?lter stones of the attachment
21, so that with each rotation of the eccentric I!
the attachment 21 is rotated through an angular
distance equivalent to the pitch of the stones and 15
then remains stationary for a certain time.‘ The
abutment ‘I8 is so arranged that it operates the
rods 08 and M of the valve 02, that is to say. opens
and closes the valve 02 during the time that the
attachment 21 stands still.
'
20
The rollers 45 are arranged on the arms III
The form of apparatus shown in the drawings is
adapted for washing nitrated starch. The acids
employed for this purpose of different concentra
tion are conducted to the containers "-4. ar
ranged on‘ the horizontal axle ‘II. The containers 25
are of triangular longitudinal section (see Fig. 8)
and the common axle ‘ll is passed through the
lowestcorner. Each container lies inside one of
to guide the latter on to the edge of the grooves 44.
An arcuate rib ll is arranged as a ?xed rail on
a part of the circular path and the height of this
containers opens at its' lowest pia‘int into one of 30
the pipes Hit-Hit. Each ‘of the tubes has a
with a swallow tail groove 44 for each of the
arms 40;
'
_
'
- These grooves form guides for the arms ll in
order to prevent side displacement by bending at
the pivots ll, when the arms 40 are raised above
or lowered to the ?lter stone.
.
' rib, which does not rotate with the attachment
the ?xed containers "-48, and each of these
straight extended end provided with holes 81, and
increases progressively from one end until the
directed radially to ‘the shaft ll, so that when
height shown in Fig. 3 is reached for the purpose the attachment stands still it is positioned in the
of raising the arm 40 at a determined position of ‘middle of one of the framu N.
its path from the ?lter stone to which it belongs,_
The axle ‘I! is mounted in bearings 08 and II
~ and then lowering it again to the same ?lter stone.
and is connected by lever I‘! and rod II with a
Rollers 41 are provided on the arm ll to guide triple lever ll, loaded at its other end by the
it along the rail 48.
‘
weight I". The triple lever is movable about the
At that part of the circular path at which the ?xed axle Ill, and its t d arm III is connected 40
frames 39 are fully raised there are provided with the lever III mova le about the axle I" by
three cleaning devices namely the screw conveyor means of the rod I II. The lever I" is provided
II which, rotating in the direction of the arrow with a roller Ill whichrolls on the periphery of
4!, cleans the ?lter stone and removes the ad
the cam I01, and is operated by the abutment I".
herent material from the stone over the edge 58
In washing nitrated starch the apparatus is 45
of the attachment into a container II. After operated as follows:— the screw conveyor there follows a series of
A reduced pressure isset up in the conduits
brushes Ii ?xed on an endless chain I0. The
chains move over rollers l2, 53, of which I!
revolves loosely and II is ?xed on to the shaft 5|.
The shaft It drives the screw conveyor 48 through
a worm gear 85 and also drives through helical
screw gear ‘I’, It, the conical brush l1 which
cleans the downwardly bent edge ll of the attach
ment. All three cleaning devices move the
material into the container II.
The material to be treated is conducted from
the container II to the separate cells formed by
each ?lter stone and frame.
The container N is in the form of a funnel,
and its lower wide opening II is closed by'a ball
valve 62.
The . valve‘ If is connected with one
end of the lever N movable about the pivot 88,
and is operated by means of the draw rod ‘I.
For this purpose the draw rod OI is'connected
with the arm ‘I of a triple lever. the second arm
61 of which through the rod II is in hinged con
nection with the beam ‘ll movable about the
pivot ll.
~
70 _ The lever ‘ll carries at its free end a roller ‘Ill.
The weight ‘II-?xed on to the third arm ‘II of
the triple lever presses on the one hand by means
of the rod I! and the lever M the valve 02 into
its seating, and on the other hand by means of the
76 lever 01 and the rod II the roller ‘Ill against?‘ the
i“ MWMMWWMWWMMMMMW
iii-2" each of which opens into a special col
lecting vessel, not shown in the drawings. The
pulplike nitrated starch is conducted to the con 60
tainer “in amounts determined beforehand. The
container Iii is ?lled with concentrated sulphuric
acid, containers "-4! with nitric-sulphuric acid
solutions. of progressively lower concentration
‘and the containers Q4, II and II with water. The 55
filling ‘of the containers is e?'ected each time be
fore the attachment is moved on through a sub
division, that is to say over one of the frames 30.
Conveniently conduits H! are provided for feed
ing the several containers in batches.
First of all the valve 02 is opened by the pro
jection ‘It, by the operation ‘of the rods I1, I‘,
85 and 84, as the lower opening SI of the con
tainer N is very wide. it empties itself suddenly
and its contents are poured over the ?lter stone 65
Ill standing under the container It. The pulp
like mass suddenly poured on the stone dis
tributes itself on" the stone in the frame standing
above it in a layer of uniform thickness.
Simultaneously the projection Ill operates the 70
rods III, ill, II, II, I’! and turns the axle 1!
in the direction of the arrow Ill so that the
contents of all the containers "-4! are poured
respectively into the funnels 80-08, and through
the tubes Ill-Ill to trickle between each two 75
o '
3
9,127,860
movements through their ?ne boreholes 91 on
From the position 399 onwards the frames 39 ‘
are raised by therib 49 so that the material can
under the tube ends. The acid or water so con-~ be removed by the conveyor devices 48 and Si.
ducted to the layers of nitro starch forms there
These conveyor devices remove the material freed
on layers of liquid of the same depth above each. » from acid to the container 59 and simultaneously
Concentrated‘ sulphuric acid flows, from the the edge of the attachment is cleaned by the
container 89 on to the empty stone 282, and is brush'i'l. Water is drawn from the stone com
drawn therethrough by the vacuum under the ing from the cleaning devices, through the slot
stone. The object of this operation is to free the 359 and the tubes 39! and 319.
The above description is given as if the ap 10
10 stone 282 from the water it contains’. This acid
is sucked off while the stone is in the position ‘paratus were at rest, but as it is moving step by
immediately following, that is to say where in step this order of procedure is repeated at each
the drawings (Fig. 4)vthe stone 283 is standing._ movement forward of the attachment so that
The channels under the stones 282 and 283 open continually a stone is covered with fresh ni
15 in the position shown in the drawings, through trated starch, and with the exception of those 15
standing under the cleaning devices, acidof the
the slot 359 of the circular body 35 into the com
mon ?exible conduit 38L The acid here drawn described different concentrations or. water is
off is regenerated.
conducted to the remainder.
"
The water required for the process as described
The fresh mass of nitrated starch falling from
is about 0.7 kilo per kilo of nitro starch.
the containers 69 comes to the stone 28L It con
20
We claim:I
' '
tains still a considerable amount of acid, which
to the ?ltered nitrated starch cakes standing
' is drawn off by the vacuum under the stone,
1. A process for the removal of nitrating acid
from nitrated starch by displacement of the acid
sitions immediately following this suction, ?l with water, which consists in drawing the water
tration of the starch occurs simultaneously on ' successively through a series of batches of the 25
stones 284- and 289. The channels 99 under the , nitrated starch on‘ ?lters wherein the liquid drawn
stones 28l, 284, and 285 open in the position of through the last ?lter of the series is passed
the attachment shown in the, drawings through into the next preceding ?lter and so on, until the ‘
slot 342 of the annular body 39 into the ?exible acid removed from the successively ?ltered
batches‘ of the series is drawn through a ?lter 3.0
conduit 382 corresponding to this slot. The con
centrated acid here drawn off is regenerated and containing fresh nitrated starch, the water
washed nitrated starch being withdrawn from
used for nitrating fresh starch.
.
The acid from the container 8| is poured on‘ that end of the series where the fresh water
to the nitrated starch lying on stone 299. This enters while the ?lter thus cleared before'being
acid has been drawn from the material on stones charged again with nitrated starch is freed 35
partly in this position, and partly in the two po
‘so
[as
‘
I
.
289, 299 and 2!“. The suction filtering is effected from water.
2. A process for the removal of nitrating acid
in the three'succeeding positions 289, 281 and
288 throughthe slot 393 and the tube 393. The I from nitrated starch by displacement of the acid
with water, which consists in drawing the water
successively through a series of batches of the ni 40
The more dilute acid from container 92 which' trated starch on ?lters wherein theliquid drawn
has been drawn from the material lying on stones through the last ?lter of the series is passed into
292, 293, and 294 is conducted to the material on the next preceding ?lter and so on, until the
stone 289. The channel 39 corresponding to acid removed from the successively,“ ?ltered ‘
batches of the seriesxis drawn‘ through a ?lter 45
46 stones 289, 299 and 29l opens through the com
mon slot 344 into the ?exible tube 399. The acid containing fresh nitrated starch, the water
washed nitrated starch being withdrawn from
drawno? here goes to stone 289 through the con
tainer 8|. The aqueous acid from container 83 that end of the series where the fresh water
which is drawn from the material on- stones ' enters while the ?lter thus cleared before being
50 296-—2 98 is conducted to ?lter stone 292. Suction charged again with nitrated starch is freed from
water by displacing the water in the ?lter with
?ltration goes on in the three succeeding‘ posi
tions 292,293 and 294 and the liquid is conducted a constituent acid of the nitrating acid.
3. A process for the removal of nitrating acid‘
through the slot 399 of the annulus 39 common
to these positions, and through the ?exible-tube from nitrated. starch by'displacment of the acid
with water, which consists in drawing the water 55
395 and the container 82 to the stone 299.
Pure water ?ows from the container 94 on to successively through a series of batches of the
the material on, stone 299. Suction ?ltration goes nitrated starch on ?lters wherein the liquid
on in both succeeding positions 295 and 298, and drawn through the last ?lter of the series is
the liquid. drawn off goes through the s1ot346 into passed into the next preceding ?lter and so on,
the ?exible tubing 369. It ‘is then conducted to until the acid removed from the successively ?l 60
container 83 from where it goes to the stone 292. tered batches of the series is drawn through a
In the same way pure water ?ows from the ?lter containing fresh nitrated starch, the water
container 85 on to the material on ?lter stone 291. washed nitrated starch being withdrawn from
Suction ?ltration goes on in the two succeeding ‘that end of the series where the fresh water
positions 291 and 298 through the slot 391 and enters while the ?lter thus cleared before being 05'
tube 381 and the liquid drawn oil’ is conducted charged again with nitrated starch is freed from
water by displacing the water in the ?lter with
to the container 83.
_
.
'
r
acid drawn of! here is regenerated and used for
40 nitrating fresh starch.
' The material on stone 299 receives pure water
from containers 99 which is drawn of! in posi
70 tions 299 and 399 through the slot 898 and the
tube 399.
,
.
sulphuric acid.
_
ALFONS xrmz. ’
JOHANN mm.
70
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