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Патент USA US2109129

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Patented Feb. 22, 1938
2,109,129 I
UNITED‘ STATES PATENT OFFICE
2,109,129
APPARATUS FOR HIGH VACUUM DISTILLA
'
TIONS
Eric William Fawcett and John Iiewis McCowen, -
Northwich, England, assignors to Imperial
Chemical Industries Limited, a corporation of
Great Britain
Application July 30, 1936, Serial No. 93,338
Inv Great Britain March 7, 1934
8 Claims. _(Cl. 202-205)
I
This invention relates to improvements in ap
paratus for high vacuum distillation; and it com
prises an apparatus organization for high vacu
horizontal surfaces;
um distillation of materials yielding upon dis
the apparatus of Fig. 1;
section and partly in elevation, of a still having
Fig. 2 is a view illustrating a modi?cation of
'
Fig. 3 is a diagrammatic view, partly in vertical 5
5 tillation at least one non-?uent component, com
prising a chamber adapted to be evacuated, - section and partly in elevation, of ‘a still having
'
means providing a hot surface in the chamber, vertical cylindrical surfaces; and
_Fig. 4 is a detail view to show the shape of
means providing a cool surface in, the chamber
‘and means in the chamber for scraping at least the scrapers in the apparatus of Fig. 3.
In the drawing, in which like reference char- 10
'10 one of said surfaces to remove materials there
from; all as more fully hereinafter set forth and acters indicate like parts, Fig. 1 shows a hori
zontal type Still. It comprises a cylindrical dis
v
.
The invention relates to the distillation under , tillation chamber Hi, the upper inner surface of
high vacuum of substances, liquid or solid, which which, indicated at H, forms the cold or con15 yield either a solid (1. e. non-?owing) distillate, densing surface. The chamber has a head l2 on
or a solid residue,_or both, and more especially one end. The upper portion of the cylinder is
to molecular distillation in which the distilling provided with a jacket I3 de?ning .a chamber [4
and having an inlet l5 and outlet I6 for circula
and condensing surfaces are in very close prox
imity, namely of the order of the mean free path . tion of cooling liquid. The cylinder is mounted
20 of the distilling molecules at the pressure within for rotation in a stationary head box ii, a suit
as claimed.
4
_
15
able ?anged, vacuum-tight rotary joint being 20
the apparatus’.
The principal object of the‘ invention is to . provided as indicated at Ill. The head box has
provide a means for overcoming the di?iculty of an outlet I9 adapted to be put in communica
removing the solid distillation products from the tion with a high vacuum pump (not shown), and
25 distilling or condensing surfaces, a difficulty an outlet 20, closed by a vacuum-tight valve in- 25
dicated at 2|, for withdrawal of condensate.
which has hitherto hindered the commercial ap
plication of the technique of high-vacuum dis~
30
The hot surface takes the form of a shallow
tillation to the treatment of solid substances or
tray 22 suitably supported adjacent the upper,
substances yielding solid products.
part of cylinder l 0 as by a bracket 23 and spaced
The present invention is 7applicable to the
treatment of initial substances whichare solid
under the distillation conditions and which yield
a solid residue or distillate under these condi
tions, i. e., a process which from one aspect may
35 be regarded as "high vacuum sublimation", also
to the treatment of substances which initially are
liquid or which are introduced to the heating
surface or surfaces incorporated with a liquid
carrier medium to form a fluent mixture, and
40 yield a solid residue or distillate.
.
The invention comprises the provision within
a vacuum distillation chamber of an intermit
from the cold surface li a centimeter or there- 30
abouts. The tray is adapted to contain a thin
layer of material to be distilled, indicated at 24.
The tray is heated by an electrical heating ele
ment indicated diagrammatically at 25 and sup
plied with current by wires 30.
'
,
Material to be distilled is introduced into the
tray through a manhole 3| hermetically closable
by a cover 32. In ?lling the tray, the manhole
is brought to the top by turning cylinder H).
In operation, material, e. g. beta-aminoanthra~ 40
quinone or other substance referred to post, is
distilled and condenses as a non-?uent crust or
tently or continuously operated scraping device the like on surface ll. Means are provided for
adapted to traverse the condensing surface (or removing the adhering condensate, comprising a
45 surfaces) on the distilling surface (or surfaces) scraper ring 33 advantageously of the type of an 45
or both, removing by scrapingso'lid material from engine piston ring and making a snug sliding ?t
in cylinder Ill. The ring has attached thereto a
the said surfaces, and depositing said solid mate
spider 34 having a central nut 35. The ring is
rial in a suitably disposed receptacle or recep
adapted to be moved axially along the length of
- tacles from which the solid material can be re
50 moved as desired.
In the accompanying drawing is shown, more
or less diagrammatically, three examples of spe
ci?c embodiments of apparatus within the pur
view of the invention. In the drawing,
55 Fig. 1 is a diagrammatic view, partly in vertical
the cylinder by means of a threaded shaft 36, 50
engaging the ‘nut and journaled in head l2 as
at 31. A reversible motor 38 mounted inside head
box I1 is arranged to drive the shaft as shown.
Upon operating the motor, the ring is caused to
move the length of the chamber I 0 and scrape 58
2
2,109,129
material towards the outlet 2|. In order to pre
tioned adjacent the lower portion of the cylinder,
vent material scraped off by'the ring from fall
as shown, and delivers through an outlet conduit
' ing back into the tray, cylinder It is rotated
60 to an outlet Si in chamber 50, valved as at 62. v
This means is for removing undistilled residue.
Scraper means are provided, comprising a
sharp-edged scraper blade ‘I engaging the sur
face of cylinder SI and mounted at top and bot
tom on rings as adapted to be supported for re
tation in an annular groove 8'! at each end» of
manually or otherwise, through a su?lcient angle
to prevent such falling back, prior to actuating
the scraper.
'
.
As an example of the use of this still, a typical
evaporative distillation operation may take from
one to two hours. Distillation is started as de
10 scribed and when a‘ thin layer of condensate
forms on surface, II to a predetermined thickness
cylinder 5|, as shown. The scraper advantage
ously has a cross-section such'as shown in Fig. 4.
which may occur every ten or ?fteengminutes,
drum II is tilted and the scraper ring set in
operation, and is moved the length of the cylin
der from left to right and then back again. The
drum is then tilted back and distillation is ref
Rings 66 are provided with rims 68 having gear
teeth. The rings are driven by‘means of two
sumed. The time required for the traverse of
the scraper may be half a minute or less, so that
the scraping time is usually negligible compared
with the operating or distilling time.
Fig. 2 shows a modi?cation'yin which periodic
tilting of the cylinder is done'away with. In this
modi?cation, a_ modified ring II is providedcut
away at the top, as shown, carried-by a spider
ll driven by shaft 36. The spider has a guide
pinions 89 mounted on a shaft ‘Ill Journaled as
at 1| in brackets 53 and extending out through 15
cylinder ill. The exposed end of the shaft is pro
vided with a handle ‘II. A vacuum-tight bearing
‘I3 is \provided to prevent leakage'around the _
shaft. Upon rotating the handle, the scraper is
caused tomove over the cold surface and remove
material adhering thereto, which falls to. the
bottom of chamber 50. If desired, shaft 10 may
be operated by an electric motor as in Fig. 1. The
apparatus is shown as also having a scraper
adapted to remove any material from the‘wall
portion 42 cooperating with a rail 43 on the lower . of cylinder 54. This is advantageous where ‘the
portion of the tray structure, so as to keep the distillation residue is non-?uent in character.
spider from rotating while allowing lengthwise Thus, a scraper bar ‘It is provided engaging cyl
motion. In this modi?cation, cylinder II is ar
inder 54 and supported from rings it by support
ranged-with an outer jacket it completely sur
ing members 15 and ‘It as shown. '
t
rounding it, so‘that the entire surface is cooled.
In operatiomcylinderll is rotated slowly and
In operation, the ‘apparatus is put under very
high vacuum through. outlet l8. Cylinder 54 is
brought to proper temperature and cooling ?uid
is circulatedv through chamber I2. Through pipe
continuously, as by a belt 45 and pulley 4i driven
by suitable slow-speed power means, not shown.
Thus condensate is continuously brought to non ‘ 51 is fed the substanceto bedistilled. Fluid mix- _
fouling position and is removed during opera ,ture flows over hot surface I4 ‘and is subject to
tion. In thismodi?cation, it is advantageous to ' evaporation in its downward course. vaporizing
operate the ring, in the outward (right-to-left) ~ constituents condense on cold sm'face II. From
' direction, at a fairly rapid rate, so that the ring time to time or continuously, handle ‘I! is turned
will not force any appreciable amount of con
to cause material to drop from the cold surface
densate outward. In practice, suitable swivel into the lower portion of chamber SI. Undis
conduit connections (not shown) are. provided tillable residue, if any, drops into collector W.
for the ?ow of cooling water to permit such cir ' From time to time, undistillable residue is taken
culation while the cylinder rotates.
'
of! through valve 82 and the distilled product is
_ The stills of Figs. 1 and 2 are wellsuited not,
only for distilling liquid materials which give.
taken oifthroughvalvellk
'
These stills- are usually made of steel or stain
less steel, and can be made in any other material
non-?uent distillates, but also for distilling ma
terials in which the raw material, the residue and
the distillate are all non-?uent.‘ Powdered solid
materials can readily be spread on the tray and
any residue scraped or- otherwise removed from
the tray after distillation is ?nished.
- In a typical process makinguse of the pres
50 having a vacuum outlet is communicating
with a high vacuum pump (not shown), and an
tion. The '?uent mixture was fed through pipe
to suit particular requirements.
"
ent invention, a quantity of crude beta-aminoan
thraquinone to be puri?ed (melting point about
298° C.) was mixed withabout an equal weight of
' Fig, 3Vshows a modification particularly well a petroleum oil which had previously been freed
adapted for continuous operation. The apparar by evaporative distillation, of all matter volatile
tus comprises a cylindrical distillationwchamber under the conditions of the evaporative distilla 55
outlet 2. with valve 2|, as in Fig. 1.
In this
' still, the cold surface takes the form of a double‘
walled cylinder 5| enclosing a chamber Hand an
outlet connection I! and outlet It for cold water
5'! of the apparatus of Fig. 3 to the hot surface, ‘
which was maintained at about 120° C.‘ A vac
uum was maintained in the'chamber of the order '
of 10-5~ mm. of mercury.'_ The cold surface in
this example was 2 cm. from thevhot surface.
or other cooling ?uid circulated through the
chamber. Thejcylinder is supported from the
distillation chamber walls by brackets 53. The
Pure beta-aminoanthraquinone ‘(melting point
hot surface takes the form of a hollow cylinder
the hot surface and were removed through out 65»
let ", together with the petroleum oil. The con- _'
54 concentric with and closely adjacent cylinder
51 and having inside it any suitable heating
311° C.) evaporated off and condensed on the
cold surface, while the impin'ities remained on
means, indicated by way of example as an elec
densate was removed by slowly rotating the
trical resistance heating coil 55 supplied by wires
scrapers.
»
In carrying out such process in the apparatus 70
70 30. The bottom of cylinder M is closed by a ta
pering cap 56 as shown. Material to be distilled of Figs. 1 and 2, the crude solid material can be
is fed in ?uent condition through an inlet pipe put directly in the tray. Condensate is removed
51 and is distributed in a thinv ?lm to the outer. by operating the scraping .ring as described. ,
surface of cylinder I4 with the aid of a conical
As examples of distillation operations to which
,16 distributor It. A funnel-like collector I! is posi the present invention may be applied with ad 76
3
mouse
vantage, may be mentioned the extraction of caf
feineifrom ground dried coffee beans, the extrac
tion of quinine from barks containing the same,
the puri?cation of crude beta-aminoanth'raqui
none, etc., in all which cases a solid distillate is
obtained which is removed according to the in
vention. In distilling these (solid) materials in
- the apparatus of Fig. 3, they are dissolved or
suspended in comminuted form in a carrier me
the chamber for scraping at least one of said sur
faces to remove materials therefrom.
'
.4. Apparatus for high vacuum distillation of
materials yielding upon distillation a non-?uent‘
distillate, comprisingv a chamber adapted to be
evacuated. means providing a hot evaporating
surfacewithin the chamber, means providing a
cool condensing surface in the chamber closely ‘
spaced'from the hot surface and adapted to re
ceive the distillate, and means in the chamber for 10
10 dium of such character as toform a ?uent mix vscrapirig?the cool surface to remove condensed
ture under the conditions of distillation; e. g.,
a linseed stand oil or a petroleum oil which has‘ material" therefrom, so as to expose the cool sur
face-for’ reception of distillate.
been previously freed of light volatiles by evapo
5. Apparatus for high vacuum distillation of
rative distillation. In the apparatus of Fig. I,
materials yielding upon distillation a non-?uent 15
15 the materials can be put directly in the tray in distillate, comprising a chamber adapted to be
comminuted form.
.
This case is a continuation-in-part of our prior evacuated, a ?at horizontal member arranged to
a hot surface and to retain a body of raw
application, Serial No. 9,873, ?led March '7, 1935. provide
material to‘ be distilled, closely adjacent means
What we claim is:
1. In a ‘molecular distillation apparatus having providing a‘ cool surface for condensing distilled 20
20
material within the chamber, and means in the
an element providing a hot surface, the combi
chamber ‘for scraping the cool surface to remove
nation of scraping means, means providing. a con
condensed material therefrom.
densing surface closely spaced from the hot sur
6. In a high vacuum distillation apparatus
face at a distance of the same order as the mean
adapted
for distillation of materials yielding a 25
- free path of molecules to be distilled, and means
non-‘fluent
distillate upon distillation and having
so constructed and arranged as to eil'ect relative
movement between said scraping means and said means providing a heated surface and a closely
cold surface vfor condensation of such ma
condensing surface so as to remove distillate spaced
terials,
the improvement comprising a member
from the condensing surface.
arranged
in contact with the cold surface and 30
2. An apparatus for effecting short path high
movable‘ with respect thereto, and means for
vacuum distillation comprising means providing moving said member over the cold surface to de-'
a cooled condensing surface, an evaporating sur
tach condensate therefrom.
face substantially parallel to the said condensing
'1. Apparatus for distillation of materials hav
surface and located a distance therefrom of the ing non-fluent components, comprising means
same order as the mean free path of molecules providing a heated surface, means providing a
to be distilled, means for distributing material to cooling surface closely spaced therefrom, means
for scraping at least one of said surfaces to de
be distilled over the evaporating surface, a scrap
ing device in sliding contact with the cooled con
tach non-?uent materials therefrom and a hous
densing surface and adapted ‘to scrape the cooled ing enclosing said surfaces and said scraping
means.
condensing surface, said evaporating and con
8. In a molecular distillation apparatus having
densing surfaces being enclosed so that they can
be maintained under high vacuum, and a recep— an element providing a hot surface, the combi
tacle for the reception of material scraped from nation of scraping means, means providing, a
condensing surface closely spaced from the hot
condensing surface.
‘
' ‘
45 the3. said
Apparatus for high vacuum distillation of surface at a distance of the same order as the
materials yielding upon distillation at least one mean free path of molecules to be distilled, and
non-?uent component, comprising a chamber means so constructed and arranged as to effect
adapted to be evacuated, means providing a hot relative movement between said scraping means
and said hot surface so as to remove residue from
evaporating surface in the chamber, means pro
.
.viding a cool condensing surface in the chamber the hot surface.
closely spaced from the hot surface and adapted
to receive the distilled component, and means in '
, ERIC WILLIAM FAWCE'I'I‘.
JOHN L MOCOWEN.
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