4901 4905.output

* GB785308 (A)
Description: GB785308 (A) ? 1957-10-23
Process and apparatus for the production of kaffir beer
Description of GB785308 (A)
PATENT SPECIFICATION
7859308 Date of Application and filing Complete Specification Sept 15,
1954.
No 26765/54.
Application made in South Africa on Oct 12, 1953.
Complete Specification Published Oct 23, 1957.
Index at acceptance:-Classes 14 ( 2), E 3; and 46, D(IG: 2 N 1: 2 N
6).
International Classification: -B 101 d C 12 b.
COMPLETE SPECIFICATION
Process and Apparatus for the Production of Kaffir Beer I, R Ic HARD
MAX HEINRICH, a citizen of the Union of South Africa, of 99,
Rustenburg Road, Emmarentia, Johannesburg, Transvaal, Union of South
Africa, do hereby declare the invention, for which I pray that a
patent may be granted to me, and the method by which it is to be
performed, to be particularly described in and by the following
statement: The present invention relates to a new and improved process
and apparatus for the brewing of kaffir beer.
The methods and apparatus hitherto employed for the brewing of kaffir
beer have been of an unscientific nature and the systems used have
been based almost entirely on the methods used in the native kraals
Thus the equipment in kafflir beer breweries in native compounds and
locations was of a primitive nature, difficult to keep clean and was
unhygienic The brewing processes employed in these breweries were many
and varied and of a rule of thumb nature, and were often without any
apparent logic, blindly following recipes handed down from generation
to generation This application of small scale native kraal brewing
methods to large scale brewing resulted in the production of kaffir
beer which is not of a high standard and with very considerable
variations in quality These primitive methods of large scale brewing,

moreover, produced kaffir beers of unpalatable flavour They were quick
souring often giving rise to harmful acidity due to the production of
acetic and butyric acids.
It is an object of the present invention to provide a novel process
and apparatus to produce a palatable kaflir beer of greatly improved
constant high quality free from or substantially free from deleterious
constituents such as acetic or butyric acids and other undesirable
fermentation products.
A further object of the invention is the acceleration of the brewing
operation and the provision of a plant of increased production
capacity and requiring a far smaller surface area of buildings as
compared with the known systems.
lPnce Other objects of the invention will become apparent from the
following description 50
In accordance with the invention, the brewing operation includes
distinct and separate stages carried out in separate reactors:(a) A
souring operation in which kaffir corn malt or other malt material
suitable for the 55 production of kaffir beer is treated in a closed
lactic acid generator with temperature control as a mash under
conditions suitable for the generation of lactic acid, while
substantially inhibiting the formation of acetic acid, buty 60 ric
acid, or like noxious acids; (b) A saccharification operation in which
product from the souring operation together with added kaffir corn
malt or other malt material suitable for the production of kaffir beer
are 65 saccharifled to maltoses and some glucose in a saccharification
vessel; (c) Straining the product of the saccharification; (d)
Fermentation of the strained product in 70 a closed fermentation
vessel so as to exclude infection The expression kaffir corn" when
used herein and in the claims denotes "Sorghum Vulgare ".
Preferably, a further distinct and separate 75 stage is interspersed,
namely a conversion operation, in which whole mealie (maize) corn,
whole kaffir corn or rapoko or other starchy or carbohydrate material
suitable for kaffir beer production is converted wholly or in part 80
into dextrin, preferably in a pressure converter The product of
conversion is then treated in the saccharification operation together
with the product from the souring operation and with added kaffir corn
malt or 85 other malt material suitable for the production of kaffir
beer.
(a) Sou RING.
In the souring stage kaffir corn malt or other malt material suitable
for the production of kaffir beer is treated as a mash under
conditions suitable for the generation of lactic acid, while
substantially inhibiting the formation of noxious acids such as acetic
acid and butyric acid The most troublesome bacteria are the acetic

acid type, because they turn the 785,30 g beer sour very quickly and
make it unpalatable sometimes even before fermentation is complete
Quite apart from the bad flavour, the acetic acid has an adverse
biological effect on the brewing process For this reason a pure
culture of lactice acid bacteria is employed.
To allow of the propagation of a pure culture of lactic acid bacteria,
a lactic acid generator is employed in which certain favourable
conditions are maintained in the mash and rigidly controlled,
preferably automatically The acid production is controlled by simple
tests and is stopped as soon as the required concentration of lactic
acid has been produced Usually for each 150 to 200 lbs of kaffir corn
malt gallons of water are employed and a temperature of between 480
and 52 C is maintained until a concentration of preferably about 1 5
per cent of lactic acid is attained.
This usually takes place in 12 to 15 hours.
At this stage, the acid production is usually arrested by boiling the
mash and thus killing the bacteria In this manner the required degree
of sourish flavour is achieved and uniform conditions are set up for
the following brewing operations The production of the pure lactic
acid cultures may advantageously be carried out on kaffir corn malt
under conditions to produce an acclimatised strain for subsequent use.
CONVERSION.
In this stage whole mealie (maize) corn, whole kaffir corn, rapoko or
other starchy or carbohydrate material suitable for kaffir beer
production is converted wholly or in part into dextrin, preferably in
a pressure converter.
The operation is preferably carried out in a pressure convertor
provided with means for the direct injection of steam and with a
plurality of tiers of dehusking and comminuting arms mounted radially
on the inside of the walls of the convertor A plurality of dehusker
blades mounted on a central rotary shaft are provided to coact with
the aforesaid dehusking and comminuting arms A concentrated mash of 30
to 40 gallons of water for each 100 lbs.
of cereal is prepared and heating is carried out b X direct injection
of steam to set up a pressure of 20 to 30 lbs per square inch gauge
The conversion is generally completed in 10 to 20 minutes after the
pressure has been set up.
Prior to the present invention, the preparation of the cereal was
carried out in open cookers in which the starch was frequently burned
to the detriment of the flavour and with loss of food values.
(b) SACCIIARIFICATION In this operation, the product from the souring
operation and preferably the product from the conversion operation
together with added kaffir corn malt or other malt material suitable
for the production of kafir beer are saccharified to maltoses and some

glucoses in a saccharification vessel.
The aforesaid conversion product and the product of souring are now
run into a saccharification vessel and may be brought up to a suitable
concentration of solids, say 12 per cent by weight, by an addition of
kaffir corn malt or other diastatic material suitable for the
production of kaffir beer.
The saccharification vessel in accordance with the present invention
which we term a " Universal Aggregate " is closed and is provided with
means, e g a coil, for the introduction of steam for indirect heating
or water for indirect cooling, as required, and a jet or jets may
further be provided for the injection of steam The said temperature
regulating coil preferably extends over the greater part of the height
of the Universal Aggregate A stirrer is provided to keep the materials
in the Universal Aggregate thoroughly mixed and to facilitate heat
transfer in heating and cooling.
The mixture is heated by direct and indirect steam injection to a
temperature and for the duration required to attain the desired degree
of saccharification Usually only part of the mash is converted into
sugars (maltose and some glucose) for example to a concentration of
about 8 % by weight, so as to limit the amount of alcohol produced in
the subsequent fermentation to not more than 3 per cent by weight as
usually prescribed by legislation or regulations relating to natives
and to retain nutrient values in the kaffir beer.
The temperature is usually maintained at between 53 and 55 C for 2
hours The mash is then slowly heated up to about 75 C to sterilize the
mesh and then cooled to about C.
(C) STRAINING.
The product is then run via a strainer for the separation of husks to
the alcoholic fer 105 mentation stage It may be advantageous to
subject both the mash prior to straining and the filtrate from the
strainer to be introduced to the fermentation vessel to a homogenising
treatment 110 (d) FERMENTATION.
The fermentation in accordance with the invention is carried out in a
closed unit so as to exclude infection by wild strains of yeast and
noxious bacteria The fermentation is 115 carried out under a slight
excess pressure, e g.
of about 4 inches water gauge For the escape of the gases of
fermentation a gas escape conduit with a water seal is provided which
has the advantage that it does not become stopped 120 up if the mash
undergoing fermentation foams over.
It is one of the characteristcis of the present invention that a pure
culture of kaffir beer dextrin splitting yeast consisting of a single
125 race of yeast free from wild yeasts is employed.
For the production of this pure kaffir beer yeast culture free of wild

yeasts, it is selecat a temperature of 28 to 300 C and sufficient of
the isolated pure culture of kaffir beer yeast is added Fermentation
is usually carried out at temperatures of 24 to 450 C, and preferably
between 30 to 40 C, and the new yeast 70 is so temperature resistant
that fermentation can be carried out even at temperatures up to 550 C
The higher the temperature, within practical limits, the higher the
rate of fermentation; in practice, depending inter alia on 75 the
temperature employed, the fermentation is completed in about 12 to 24
hours.
On completion of the fermentation, the kaffir beer can be withdrawn
and is ready for consumption 80 The invention and how it may be
carried out in practice will be further described and ascertained by
way of example with reference to the accompanying drawings in which
Fig 1 illustrates in diagrammatic elevation, in part 85 in section a
plant in accordance with the invention for the production of kaffir
beer It should be understood that the invention is not limited to the
example given Fig 2 is a side elevation, in part broken away, on a
large scale 90 of a strainer in the plant assembly.
Referring to the drawings: 1 is a lactic acid generator which is
provided with a heating and cooling coil 2 through which steam or
cooling water can be passed 95 as required It is further provided with
a stirrer 3 operated by the motor 4.
is la pressure convertor consisting of a closed tank provided with 4
tiers each containing 4 to 6 teethed dehusking arms 6 100 radially
attached to the interior surface of its side wall Furthermore, a
vertical rotary shaft 7 operated by an electric motor and bevel gear 8
is provided, on which shaft 7 dehusking beaters 9 are mounted which
coact with the 105 stationary dehusker arms 6 Steam jets S, are
provided near the base of convertor 5.
is a " universal aggregate " in which the mash is saccharified to the
desired extent and is prepared for the fermentation stage 12 and 110
11 are conduits leading from the bases of the lactic acid generator 1
and the pressure convertor 5 respectively into the universal aggregate
10 13 is a temperature regulating coil extending over a greater part
of the height of 115 the universal aggregate 10 and into which steam
may be admitted for heating and water cooling Steam may further be
directly injected through the steam jet or jets S, A stirrer 14 is
provided which in its rotation 120 covers practically the entire area
of the base of the aggregate 10 and further has arms 15 which in
operation cover the lower portion of the side walls of the aggregate A
man-hole 16 for filling the aggregate and an exhaust 17 125 for the
removal of vapours are provided in the cover of the aggregate 10
Stirrer 14 is operated by an electric motor and bevel gear indicated
at 18 Conduit 19 is provided for the removal of saccharified mash from

the base 130 tively cultivated from kaffir beer wort by constant
repeated selection of those races giving the strongest fermentation
under kaffir beer brewiing conditions.
This is, for example, effected by preparing layers of agar with kaffir
beer wort e g of 9 to 14 per cent strength, about 12 per cent strength
and yeast water and growing yeast colonies thereon under conditions
favouring their growth The apparently most virile colony is
transplanted onto fresh sterile agar plates and the operation repeated
until a pure kaffir beer mono-racial yeast culture free from other
yeasts is obtained.
In order to ensure that pure mono-cultures are obtained, it is
advisable finally or at a later stage to use the drop culture method
by preparing dilute liquid dispersions and isolating individual cells
in drops taken therefrom and checked under the microscope and further
checked according to virility in fermentation, so as finally to
cultivate from an individual cell selected because of its capacity for
optimal cymase production under kaffir beer brewing conditions the
pure yeast.
The selected pure yeast race is then propagated further under
production conditions, great care being taken to keep the strain pure
and exclude intctions by wild strains of yeast and noxious bacteria
Molasses are then preferably employed as the main nutrient together
with other substances for the maintenance of the fermentive power to
the yeast Such other substances are e g yeast water from the same
strain of yeast and kaffir corn mash extracts.
The employment of molasses is of particular importance also from the
economic angle.
By gradually raising the temperatures employed in the propagation of
successive generations of the pure yeast cultures, strains are
obtained which are highly efficient at fermentation temperatures of 27
to 39 C with an optimum fermentive action at around 350 C.
Again, by propagating successive generations of the pure strains in
acid media, pure yeast cultures are produced that have good fermentive
activity in a range down to p H 3 7 and at an operational p H of about
3 9 This is of vital importance for the production of kaffir beer in
which the lactic acid contents plays such an important part in the
flavour and wholesomeness of the beer.
The yeasts in accordance with the present invention can be prepared in
a dried or compressed form for delivery to kaffir beer breweries.
Sufficient quantities of the said kaffir beer yeast are introduced,
that from the start this yeast outgrows any other species that might
have been accidentally introduced, thus assuring a uniform high
standard of kaffir beer.
In the brewing operation, the mash is preferably introduced into the

fermenting vessel S -78 D,3 M of aggregate 10 through a homogeniser 20
and a pipe 21 controlled by valve 22 to the feed tank 23 of a strainer
24, which in accordance with the invention, embodies several novel
characteristics.
The strainer 24 (Fig 2) comprises a tapered screw conveyor 25 rotating
in a suitably supported strainer of sheet material 26 of
frustroconical shape, contained in a casing adapted to receive the
Liquid slurry expressed through the strainer 26 The latter may consist
of slotted stainless steel sheet The husks and the like are expelled
by the conveyor 25 A conduit 28 leads to a homogenizer 29 whence a
feed pipe 30 leads to near the top of the closed fermentation tank 31.
Tank 31 is provided at its top with a gas escape conduit 32 leading to
a liquid seal 33.
34 is a coil for regulating the fermentation x O temperature An outlet
pipe 35 for the removal of the finished beer is provided at the bottom
of fermentation tank 31.
All parts of the apparatus coming into contact with the materials to
be treated should be made of materials completely resistant to
corrosion under the operating conditions, e g.
stainless steel.
The apparatus may for example be operated as follows: A mash of 180
lbs of kaffir corn malt per gallons of water is filled into the lactic
acid generator 1, seeded therein with a pure culture of lactic acid
bacteria and is maintained at a temperature of about 500 C for 12 to
15 hours until a concentration of 1 5 per cent lactic acid is
attained.
Simultaneously for each 100 lbs of whole mealie corn, 30 to 40 gallons
of water are added and the mixture is treated in the high pressure
convertor 5 under a pressure of 20 to 30 lbs gauge per square inch set
up by direct steam injection while rotating the blades 9 to hydrolise
the starch and dehusk the material Under the said pressure, the
conversion takes place in 10 to 20 minutes The mashes from convertor 5
and the lactic acid generator 1 are introduced through conduits 11 and
12 respectively into the universal aggregate 10 and are made up
therein with water and kaffir corn malt to a concentration of 12 per
cent by weight of solids The mass is then brought to a temperature of
about 54 ' C by direct and indirect steam injection until a
concentration of about 8 % maltose with some glucose is attained which
is usually the case in about 2 hours The temperature is then brought
up to about 75 C for sterilising the mash whereupon it is quickly
cooled to about 300 C.
The mash is then withdrawn through conduit 19 and pumped through the
homogeniser and conduit 21 to the strainer 24, the husks and like
solids are expelled by the worn conveyor 25 whilst the slurry pressed

out through strainer sheet material 26 passes via the homegeniser 29
via feed pipe 30 into the closed fermentation tank 31.
The mash in the fermenter is seeded with a sufficient quantity of the
aforementioned isolated pure culture of kaffir beer yeast and 70 is
fermented therewith while maintaining a temperature of between 24 and
40 C preferably about 35 C Depending on the temperature, the
fermentation is completed in 12 to 24 hours and the beer is withdrawn
and is 75 ready for consumption.
It is advantageous to maintain a p H of down to about 3 7 and
preferably about 3 9.
A palatable kaflir beer of high uniform quality with a good foam and
free from 80 noxious acid is thuls produced.
A strainer in accordance with the invention comprises a frusto-conical
screen 26 (Fig 2) and a conical worm conveyor 25 therein.
The axis of the conveyor is preferably on 85 an inclined plane and the
solids from which liquids have been separated are expelled through an
orifice 36 at the upper end of the strainer, which is adjustable by a
cone 37 which can be inserted into the said orifice to 90 any desired
extent by rotation of the threaded rod 44 by means of the handle 45.
The liquid or slurry is strained through the screen 26 preferably made
of slotted stainless steel sheet into a casing 27 discharging into 95
the effluent tube 28.
The elongated axis 38 of the worm conveyor is journalled in an
adjustable pressure bearing 39.
The worm conveyor is actuated from an 100 electric motor 40 controlled
from the switchbox 46, or other suitable prime mover, via a
transmission 41 and a gear box 42.
The material to be fed to the strainer is introduced into a flat
funnel-shaped feed tank 105 23 which discharges through pipe 43 into
the interior of strainer 24.
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* GB785309 (A)
Description: GB785309 (A) ? 1957-10-23

Improvements in centrifugal pumps
We, RHODES, BRYDON & YOUATT LIMITED,
a British Company, of Waterloo Engineering Works, Gorsey Mount Street,
Stockport, Cheshire, do hereby declare the invention, S for which we
pray that a patent may be granted to us, and the method by which it is
to be performed, to be particularly des-
cribed in and by the following statement:-
This invention relates to centrifugal pumps and has for its object to
provide an improved simplified construction of twostage pump.
The invention consists in a two-stage centrifugal pump comprising a
double inlet impeller having blades projecting from both sides of a
central disc upon the pump driving shaft, and a ring having guide
vanes on its opposite sides around the impeller for the deliveries of
the first and second stages, the pump suction or inlet pipe
communicating with one side of the impeller where liquid is fed to the
centre of the disc on to the inlet tips of the blades at such side,
the delivery from this side being led via ports in the ring having
guide vanes therein, to the centre of the opposite side of the
impeller and to the inlet tips of the blades at such side, and the
delivery from such blades passing through the guide vanes into an
annular concentric or volute form passage communicating with the pump
delivery branch.
Referring to the accompanying explanatory drawings: Figure 1 is a
sectional elevation of the upper part of a two-stage centrifugal pump
constructed in accordance with this invention.
Figure 2 is a side view of the ring of guide vanes around the impeller
in Figure 1.
We utilise a double inlet impeller having blades a, b projecting from
both sides of a central disc c secured upon the pump driving shaft d,
The blades may be shrouded or of the open type The pump suction or
inlet pipe e communicates with one side of the impeller, where liquid
is fed to the centre of the disc c on to the inlet tips of the blades
a at such side The delivery from this side of the impeller passes
through guide vanes p' in a ring p arranged around the impeller, such
ring having ports q for the crossover flow between the first and
second stages of the pump The liquid is passed to the centre h of the
impeller of the second stage and then via the vanes p 2 in the ring p

to the passage i which may be of either concentric or volute form and
communicates with the delivery branch j of the pump.
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* GB785310 (A)
Description: GB785310 (A) ? 1957-10-23
Pipe couplings
A high quality text as facsimile in your desired language may be available
amongst the following family members:
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The EPO does not accept any responsibility for the accuracy of data
and information originating from other authorities than the EPO; in
particular, the EPO does not guarantee that they are complete,
up-to-date or fit for specific purposes.
PATENT SPECIFICATION
Inventor: LEWI 1 S MERVYN CECIL SEAMARK 785,310 Date of filing
Complete Specification (under Section 3 ( 3) of the Patents Act,
1949): Oct 17, 1955.
Application Date: Oct20, 1954 No 30277/54.
Application Date: Nov8, 1954 No 32324/54.

Complete Specification Published: Oct 23, 1957.
Index at acceptance:-Class 99 ( 1), G( 4 G: 29).
International Classification:-F 061.
Pipe Couplings We, PIDCO LIMITED, of Candlewick House, 116-126 Cannon
Street, London, E l C 4, a British Company, do hereby declare the
invention, for which we pray that a patent may be granted to us, and
the method by which it is to be performed, to be particularly
described in and by the following statement: -
The invention relates to pipe-couplings.
According to the invention, a coupling device for plain-ended pipes,
the ends of which are spaced:apart to permit of limited axial
movement, comprises a member stationarily mounted at the end of each
of the pipes to be coupled, to present a series of circumferential
projections on each pipe end, and a locking ring mounted so as to span
the endis of the pipes to be coupled and formed to engage said
projections by a rotational movement of said ring relatively to said
projections.
The members may each 'be formed as a clamp having an arcuate part
surrounding the pipe and, a pair or pairs of radially extending
co-operating bosses or lugs at the ends of the arcuate part bored to
receive a screw bolt or the equivalent, whereby pressure may be
applied to bring the ends of the arcuate part into closer engagement
and thus tighten the clamp around the ends of the pipe On the inner
surfaces the members may be formed with a friction lining such as, a
rubber or like substances, or with teeth or serrations.
On the outer peripheral, surface, members may b:e formed with a
circumferential series of clutch members or dogs with tapered or
inclined faces adapted to be passed through gaps formed at
corresponding positions in the end faces of the locking ring and then
to be twisted through an angle, so that the clutch members or dogs
engage frictionally in recesses of corresponding form,, provided in
the ring.
A positive lock in the form of a radially extending pin or bolt may be
provided to pass through a hole in the locking ring and, between the
clutch members or ddogs of the member.
The locking ring is formed to leave an annular space to surround the
projecting ends of the pipe and with an inwardly projecting annular
flange at a middle position and servdng as a confining element for
sealing ring 50 packings which are mounted in the spaces so formed on
each side of the annular member.
The packing may be a resilient packing material such as rubber or the
like.
The invention further comprises the features 55 of construction

hereinafter described, The invention is diagrammatically illustrated
by way of example in' the accompanying drawings, in which: Figure 1 is
a sectional side elevation; 60 Figure 2 is a corresponding end
elevation Figure 3 is a part sectional side elevation of a modified
construction, and Figures 4 and 5 are sectional side elevations of
modified constructions 'of the member and 65 its method of attachment
to the ends of the pipes to be coupled In carrying the invention into
effect according to the construction illustrated in Figures 1 and 2 of
the drawings, the pipe coupling 70 for clamping together the ends of
two pipes comprises members 1 each of angular form and provided as a
circular strap, with adjacent ends of the strap formed with radially
'extending lugs or bosses 2 and bored at co 75 incident positions at 3
' to receive a screw bolt, pin or the like 4 To assist in preventing
withdrawal of the pipes in an axial direction, the inner surface of
the circular strap is, formed with teeth or serrations 5 formed to
grip into 80 the pipe on tightening of the bolts or pins 4.
The members or straps 1 are mounted on the pipes at a determined
distance from the ends so as to leave the projecting ends of the pipes
unencumbered 85 On the outer periphery of each gripping member 1 is
formed, a circumferential series of projections, clutch members or
dogs 6 angularly spaced around the member 1 (Figure 2) at a position
near to 'but spaced from the 90 inner end face of the member.
Provided to span the ends of the pipes at the joint and to engage the
members 1 mounted on the pipes, in the manner of a bayonet joint, is a
locking ring or cylinder 7 formed as an integral unit of two identical
halves The locking ring 7 is formed with angularly spaced gaps S at
corresponding positions at the respective ends to receive the
projections or clutch members 6 of the members 1, and with recesses 9
on the inner peripheries of a form corresponding to that of the
projections or clutch members 6, for example, tapered, so that on
relative rotation of the members 1 and the locking ring or cylinder 7
the members 6 engage frictionally in the recess 9.
At the middle of the rings 7 on the inner surface is provided an
inwardly extending annular partition member 10, and in the spaces 11
provided one on each side of the partition member 10 and each
delimited by the end face of the member 1, the inner surface of the
locking ring,7, the outer surface of the projecting unencumbered end
of the pipe, and a side face of the annular partition member 10, is
mounted a sealing ring 12 of rubber or like substance The members 1
are mounted on the ends of the tubes so as to leave considerable
tolerances at the end faces, whereby the pipe ends may be effectively
coupled even with the pipes positioned, as when passing round a bed or
over uneven ground, at an angle to each other.
On the outer periphery of the ring 7 a boss may be formed with a

cylindrical recess to receive the end' of a tommy-bar for applying a
rotational movement to the ring when mounting it in position or when
undoing the joint.
In mounting the coupling, the members 1 are disposed one on each end
of the pipes to be coupled at a determined distance from each end of
the pipe to leave projecting ends, and the members tightened on the
pipes by screwing up the nuts on the screw bolts 4 to cause the teeth
on the under surface of the members to bite into the outer peripheral
surfaces of the pipe ends.
Rubber sealing rings 12 formed to a diameter slightly greater than the
height of the space between the undersurface of the ring 7 and the
outer periphery of the projecting end of the pipe are then mounted on
the unencumbered ends of the pipes to be coupled.
The ends of the pipes so fitted with members are then engaged by the
locking ring 7 which is partly rotated as by means of a tommy bar to
cause engagement of the projections or clutch members 6 in the
recesses or slots in the locking ring.
Positive locking together of the members and the locking ring is
effected by means of a set screw 16 or by similar means.
In a modified construction, as illustrated in Figure 3 of the
drawings, the inner peripheral surfaces of the members may be formed
with an annular ring or rings 17 of, for example, rectangular section
adapted to be received in a recess or recesses 18 of corresponding
form provided at the appropriate positions in the outer peripheral
surfaces of the pipe ends to be coupled 70 The members 1 may be formed
in two halves, secured together as by bolts or the like advantageously
at two diametrically opposite positions, the bolts passing through
aligned holes formed in correspondingly disposed 75 lugs formed at the
respective ends of the halves of the members 1.
In the modified construction illustrated in Figure 4 of the drawings
the members are screw-threaded on the undersurface for part of 80
their length for engagement with the correspondingly screw-threaded
end of the pipe to be coupled, the member in such case being formed as
a complete ring to surround the end of the pipe to be coupled 85 In
the modified construction illustrated in Figure 5, the members are
welded to the ends of the pipes to be coupled The members may
alternatively be shrunk on to the ends of the pipes 90 The coupling
may be made of metal, such as steel, or of a plastic It is
particularly adapted for use as a coupling for plastic-piping, which
may be made anti-corrosive, in which case the coupling may also be
made of the 95 same material.
No limitation is, however, made as to the material from which the
coupling may be made.

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* GB785311 (A)
Description: GB785311 (A) ? 1957-10-23
Manufacture of combustible gas
DE1009344 (B) FR1136956 (A)
DE1009344 (B) FR1136956 (A) less
PATENT SPECLIFICATION
lavenoir: -JACK MALCOLM HAWES.
Date of filing C'ombplete Specification: Oct 1 i, 1955.
App I licationi Dafe: Nov 12, 1954 No 32799/54.
Complete Specification Putlished: Oct 23,1957.
Inidex at Acceptance-Class 55 ( 2), D 2 G.
International Classificaltion:-Cl Ob.
COMPLETE SPECIFICATION.
Manufacture of Combustible Gas.

We, HUMPHREYS & GLASGOW LIMITED, a British Company, of Humglas House,
Carlisle Place, London, S W 1, do hereby declare the invention, for
which we pray S that a patent may be granted to us, and the method by
which it is to be performed, to be particularly described in and by
the following statement: -
This invention is concerned with the manufacture of combustible gas
from fluid hydrocarbons by a cyclic process of the kind in which each
cycle of operations comprises two main phases, namely: (a) a
gas-making phase in which the fluid hydrocarbon is cracked or reacted
with steam, which may if desired be mixed with other oxidising
gasification medium, in a gas-making chamber containing a contact bed
or mass of catalyst or refractory, and (b) a plantheating phase in
which hot plant-heating gases are passed through the plant to heat it
up for the gas-making phase which is to follow The reactions in the
gas-making phase are generally endothermic and, particularly when
heavy oils are used as the fluid hydrocarbon, solid carbon deposits
are left in the gas-making chamber or in a preliminary vaporizing
chamber In the plant-heating phase, oxygen in the plantheating gases
burns away the carbon deposits.
Prior Patent Application No 4851/54 (Serial No 751,510) outlines a
process of the kind described above in which equipment such as a
waste-heat boiler may be used to recover sensible heat in the gases
leaving the gas-making chamber during plant-heating phases, before
those gases pass to a waste stack, or under some circumstances from
plant-heating gases leaving a combustion chamber Drior to entering the
gas-making chamber Prior Patent ApplicalPrice 3 s 6 d l tion No
9813/54 (Serial No 753,051) outlines a process of the kind described
above in which oxygen-containing plant-heating gases to be used for
carbon-burning, are heated by heat-exchange with plant-heating gases
of lower oxygen content resulting from carbon burning.
According to the present invention, a process of the kind referred to
for the manufacture of combustible gas from fluid hydrocarbons is
characterised in that during plant-heating phases part of the waste
gases from the gas-making chamber is passed to a waste heat boiler
while another part of the waste gases from the gas-making chamber is
passed through a heat exchanger, air for combustion for plant-heating
being passed through the heat exchanger and heated by heat exchange
with the waste gases passing therethrough.
The main advantage of this process is that it allows excess of waste
heat not required for steam raising to be recovered and returned to
the process, thus giving a balance with just the required amount of
steam, the flow of waste gases through the waste heat boiler and the
heat exchanger being adjusted suitably.
If desired, the whole or part of the waste gases leaving the waste

heat boiler may be passed through the cooler part only of the heat
exchanger.
Preferably, during plant-heating phases, fuel (such as fuel oil) is
burnt in -a combustion chamber and the air heated in the heat
exchanger being passed to the combustion chamber and the products of
combustion passing to the gas-making chamber Part of the air may
provide primary air for combustion of the fuel oil.
the remainder of the air being introduced at a position such as to
provide excess 75,5311 65.
8 () 785,311 oxygen in the hot gases (and if necessary to complete the
combustion of the fuel oil).
Such an arrangement is described in prior British Specification No
751,510.
; The invention also provides apparatus for carrying out a process of
the kind referred to for the manufacture of combustible gas from fluid
hydrocarbons, which apparatus is provided with a waste heat boiler, a
heat to exchanger and means for passing part of the waste gases
leaving the gas-making chamber during plant-heating phases through the
waste heat boiler and part through the heat exchanger, means being 1;,
provided for simultaneously passing air for combustion for
plant-heating through the heat exchanger.
The following is a description, by way of example, of methods of
carrying out the 2 lo invention, reference being made to the
accompanying diagrammatic drawings in which:Figure 1 shows one form of
apparatus for performing a process of the kind referred to; Figure 2
shows a modified form of apparatus; and Figure 3 illustrates an
alternative form of apparatus.
3 o In both Figure 1 and Figure 2, there are shown a gas-making
chamber 10, a combustion chamber 11, a waste-heat boiler 12, a heat
exchanger 13 and a gas washer 14.
During the plant-heating phases, the hot 3.5 products of combustion
leave the combustion chamber 11 and are passed through the gas-making
chamber 10, burning off any carbon deposits Part of the waste gases
leaving the gas-making chamber 10 are 401 passed through a conduit 15
to a heat exchanger 13 and on to a waste stack, the remainder of the
waste gases is passed through a conduit 16 to a waste heat boiler 12
and then to a waste heat stack 17 which 4 a may conveniently be the
same stack as that for the waste gases from the heat exchanger 13
Valves 18 and 26 are provided in the conduits 15 and 16 to vary the
flow of the gases as required The conduit 16 to the f waste heat
boiler 12 has a branch conduit 19 leading to a gas washer 14, and a
valve and stack valve 27 are provided so that during gas-making phases
the make gas can be passed to a gas holder via the gas washer .,, 14
and other gas cleaning equipment.

In a modified arrangement shown in Figure 2, a valved conduit 21 is
provided for leading waste gases leaving the waste heat boiler 12 to
an intermediate position i-t in the heatexchanger 13 so that they pass
through the cooler part of the heat exchanger, thereafter passing to
the stack.
Adternatively as shown in Figure 3 two separate heat exchangers 22 and
23 may be provided through which air is passed in series, waste gases
from the waste heat boiler are passed through the first heat exchanger
encountered by the air (i e heat exchanger 23) and waste gases direct
from the gasrmaking chamber 10 are passed 70 through the other heat
exchanger 22.
In each arrangement, air is passed through the heat exchanger or
exchangers during plant-heating phases and then through a valved
conduit 24 to provide primary air -a for an oil burner in the
combustion chamber 11 Part of the air is by-passed through a valved
conduit 25 to provide secondary or diluent air in the combustion
chamber.
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* GB785312 (A)
Description: GB785312 (A) ? 1957-10-23
Improvements relating to hydrocatalytic desulphurisation processes
BE543447 (A) FR1143211 (A)
BE543447 (A) FR1143211 (A) less

PATENT
KS 1 -EC IWF 1 C A T O N
Date of filing Complete Specification Dec 7, 1955.
Application Date Dec 8, 1954.
No 35526/54.
Index at Accertance:-Classes 1 ( 1), AS(AIA: B 2 A: B 2 X); and 91, 02
C.
International Classification: -a Olj Cl Og.
Improvermrents relatirg to H-ydrocatalytic Desulphurisation Processes
ERRATA SPECIFICATION NO, 785 312.
Page 1, line 87, for "through out" read "throughout".
Page 3, Recycle rate, for " 100 " read " 1000 ".
Page 3, line 16 after "reactor' insert "constant".
Page 3, line 17, for "residue" read "residence".
Page 4, line 119, for "cource"' read "course"'.
Page 5, line 83, for "-100 " read " 100 ".
THE PATENT OFFICE, 28th Aprils 958 DB 04462/2 ( 7)13604 50 4/58 R Such
a process is described in British -Patents Ncs 654,152, 663,038,
669,536, 669,552-3, 679,175, 697,222, and 697,226 A particularly
effective catalyst for use in the autofining process consists of or
comprises the oxides of cobalt and molybdenum deposited on or
incorporated with a support consisting essentially of activated
alumina, said catalyst containing a minor amount of fluorine This type
of catalyst is especially effective when operating the autofining
process under equilibrium pressure conditions in which the hydrogen
derived from the feedstock is recycled to the reaction zone and the
pressure therein allowed to rise until an equilibrium pressure is
established Such a process is described in British Patent No.
lPrice 3 s 6 d l the fluorine throughout the catalyst mass It has been
found that maximum desulphurization is only obtained when such even
distribution of fluorine is achieved The fluorine content of the
catalyst may initially be distributed evenly throughout the catalyst
mass, but regeneration of the catalyst causes an overall loss of

fluorine and an uneven distribution of fluorine through out the
catalyst mass, and although additional fluorine may be added to the
catalyst in various ways it is difficult to ensure even distribution
of such added fluorine when operating with a fixed catalyst bed.
The principal object of the present invention is to provide a method
of operating the e 4,-p 1,)T 1 785,312 ?A 1.
? j ' MS Q j j _z, C 2,_ B PATENT S? 3 CIFICATION 7859312 Date of
filing Complete Specification Dec 7, 1955.
Application Date Dec 8, 1954.
No 35526/54.
Index at Acceptance: -Csses 1 ( 1), A 3 (AIA: B 2 A: B 2 X); and 91,
02 C.
International Classification: -301 j Clag.
Improvements relating to Hydrocatalytic Desulphurisation Processes We,
THE BRITISH PETROLEUM COMPANY LIMITED (previously known as
Anglo-Iranian Oil Company Limited), of Britannic House, Finsbury
Circus, London, E C 2, a British Joint-Stock Corporation, and
FREDERICK WILLIAM BERTRAM PORTER and ERNEST CARLTOX HOUS Am, both of
the Company's Research Station, Chertsey Road, Sunbury-on-Thames,
Middlesex, and both of British Nationality, do hereby declare the
invention, for which we pray that a patent may be granted to us, and
the method by which it is to be performed, to be particularly
described in and by the following statement: -
This invention relates to the hydrocatalytic process for the
desulphurisation of hydrocarbon materials, particularly petroleum
hydrocarbons, wherein the hydrocarbons are contacted at elevated
temperature and pressure with a sulphur-resistant hydrogenation
catalyst in the presence of hydrogen whereby organically combined
sulphur contained in the hydrocarbons is converted into hydrogen
sulphide which may be readily removed from the treated hydrocarbons.
A recent development of the hydrocatalytic desulphurisation process is
known as the autofining process in which the hydrogen required for the
conversion of the organically combined sulphur into hydrogen sulphide
is obtained by controlled dehydrogenation of the feedstock.
Such a process is described in British Patents Ncs 654,152, 663,038,
669,536, 669,552-3, 679,175, 697,222, and 697,226 A particularly
effective catalyst for use in the autofining process consists of or
comprises the oxides of cobalt and molybdenum deposited on or
incorporated with a support consisting essentially of activated
alumina, said catalyst containing a minor amount of fluorine This type
of catalyst is especially effective when operating the autofining
process under equilibrium pressure conditions in which the hydrogen

derived from the feedstock is recycled to the reaction zone and the
pressure therein allowed to rise until an equilibrium pressure is
established Such a process is described in British Patent No.
lPrice 3 s 6 W.
697,083 The fluorine-containing catalyst seems to have increased
dehydrogenating activity, thereby enabling a higher equilibrium
pressure to be reached resulting in increased desulphurisation.
The autofining process has been successfully operated using fixed beds
of granular and pelleted catalyst, and although satisfactory
desulphurisation has been obtained over a wide range of petroleum
feedstocks, up to and including gas oils, particularly when operating
at equilibrium pressure, the fixed bed method of operation suffers
from the following disadvantages: 1 Variable, and at times high,
recycle rates were necessary.
2 Variable plant pressures occurred and the equipment had to be
designed for the highest pressures encountered even though they were
only maintained for a short time.
3 The sulphur content of Ithe produdt varied during the course of a
run.
4 It was necessary, periodically, to take the unit off stream and
regenerate the catalyst.
Precautions had to be taken to ensure an even distribution of fluorine
during the life of the catalyst.
Various method of preparing fluorine-containing catalysts of this kind
are described in British Patent No 719,627, but there is always a
difficulty in ensuring even distribution of the fluorine throughout
the catalyst mass It has been found that maximum desulphurization is
only obtained when such even distribution of fluorine is achieved The
fluorine content of the catalyst may initially be distributed evenly
throughout the catalyst mass, but regeneration of the catalyst causes
an overall loss of fluorine and an uneven distribution of fluorine
through out the catalyst mass, and although additional fluorine may be
added to the catalyst in various ways it is difficult to ensure even
distribution of such added fluorine when operating with a fixed
catalyst bed.
The principal object of the present invention is to provide a method
of operating the 7 _ rag 7 i ^,,'/-:,', 1,7'; 785,312 autofining
process which avoids the abovestated disadvantages.
According to the present invention, a process for the autofining of
petroleum hydrocarbons, comprises passing said hydrocarbons at an
autofining temeperature and pressure to a reaction zone, wherein they
are contacted in the presence of recycled hydrogen with a fluidised
bed of a catalyst consisting essentially of the oxides of cobalt and
molybdenum incorporated with a support consisting essentially of

activated alumina, and containing between 0.1 % and 6 0 % by weight of
combined fluorine, withdrawing catalyst from said reaction zone and
passing said withdrawn catalyst to a regeneration zone, regenerating
said withdrawn catalyst, returning the regenerated catalyst to the
reaction zone, and recovering hydrocarbons of reduced sulphur content
from the products of the reaction zone The fluorine content of the
catalyst is preferably between 2.5 and 6 0 % by wt.
The catalyst may be regenerated continuously in the manner common in
catalytic cracking and other fluidized processes, or a part of the
catalyst may be regenerated periodically.
The method of operation according to the invention overcomes the
problem of fluorine distribution since the catalyst is at all times,
whether in the reactor or in the regenerator, in the form of a single
homogeneous fluid phase At the same time, constant catalyst activity
is maintained which, in turn, results in constant pressures, recycle
rates and sulphur contents of products In addition it has been found
that the catalyst is more active in the fluidized state than it is
when in the form of pellets such as have been used hitherto.
Temperature Space velocity Recycle rate Pressure In the following
table the contents obtained in this 01 pared with those obtained M
feedstock was processed over same catalyst in the form a.
the same temperature, weir velocity and recycle rate:% wt sulphur in 1
Hours on stream 25 5 ( Fixed bed 0 09 0 1 Fluidized bed 0 01 O ( In
the following example, tent of the product was kep intermittent
addition of fri withdrawal of spent catalyst.
The temperature must be high enough to effect adequate
desulphurisation and is generally between 700 and 8005 F, while the
pressure is advantageously allowed to reach equilibrium.
The following example in which no catalyst was withdrawn for
regeneration illustrates the superiority of the fluidized catalyst
over the same material in the form of 5/ljn pellets.
EXAMPLE 1.
The reactor was charged with 630 grammes of catalyst ( 72-150 B S S
mesh size) having the following composition.
Constituent % wt.
Co O 2 7 Mo O, 15 5 Fluorine 3 3 AO 2, 78 5 The catalyst was heated at
780 F in a recycle stream of hydrogen ( 720 SCF/hr /CF of catalyst)
adding fresh hydrogen to maintain a pressure of 100 p s i ga until no
more hydrogen was being consumed by the catalyst A previous experiment
in glass apparatus had established that at the linear velocity
obtained under these conditions ( 0 3 feet per second) the catalyst
was in a fully fluidized state.
The reactor was equipped with a ball valve at the inlet, to prevent
catalyst entering the preheater, and with a ceramic filter on the

exit.
A gas oil having a specific gravity of 0 844, a sulphur content of 1
29 wt, and a boiling range from 250 to 350 C, was processed over the
catalyst under the following conditions:790 F.
1 93 weight of oil/weight of catalyst/hour 2000 SCF/B set at an
initial pressure of p s i ga.
Initial-100 p s i ga.
Equilibrium-500 p s i ga.
residual sulphur EXAMPLE 2.
3 eration are corm A reactor was charged with 3600 g of then the
identical microspheroidal catalyst (average particle size a fixed bed
of the 52 5 A) with the following composition:If pellets, at
Constituent % wt 100 ght hourly space Co O 2 7 Mo O, 19 1 Fluorine 3 5
products A 03 74 7 100 The catalyst was heated at 780 F in a re 105
cycle stream of hydrogen ( 720 SCF/hr /CF of 18 0 32 0 36 catalyst),
adding fresh hydrogen to maintain a 0 0 02 0 05 pressure of 100 Dsig
until hydrogen consumption ceased.
the sulphur con A Kuwait gas oil having a specific gravity of 110 t
constant by the 0 844, a sulphur content of 1 29 %, wt and a -sh
catalyst and boiling range of 2500 to 3500 C, was processed over the
catalyst under the following conditions: 785,312 Temperature Pressure
Space velocity Recycle rate The linear velocity of the gases for these
conditions was 0 15 feet/second This rate was found, by experiments in
glass apparatus, to be sufficient to fluidise the catalyst.
As the run proceeded, the sulphur content of the product rose until it
reached 0 1 %+ weight At this stage, fresh or regenerated catalyst was
added to the reactor at a rate of 12 2 g /hr Spent catalyst was
withdrawn at the same rate to keep the level in the reactor This was
equivalent to a catalyst residue time of 295 hours.
It was found that this residence time was sufficient to keep the
sulphur content of the product constant at 0 1 % wt Under these
conditions the pressure and the recycle rate were constant at 260 p s
i ga and 2400 SCF/B respectively The carbon content of the spent
catalyst was 20 % wt.
Production of 0 1 % wt sulphur gas oil was continued for 450 hours at
which stage the run was terminated The catalyst was withdrawn from the
reactor in zones, and each zone was analysed for fluorine content It
was found that the fluorine content of the catalyst was 3.5 % wt in
each zone.
Catalyst Space velocity Catalyst temperature Pressure Gas recycle rate
Catalyst residence time Carbon on catalyst Linear velocity of gases
The catalyst may be regenerated continuously at elevated pressure, and
in this case the catalyst is passed between the reactor and
regenerator in the manner commonly employed in fluidized catalytic

processes such as fluid, hydroforming and fluid catalytic cracking.
Regeneration, may in this case, be carried out under the following
conditions:Catalyst temperature 10500 F.
Pressure 300 p s i ga.
Catalyst residence time 5-10 hours Carbon content of regenerated
catalyst 0 1 % wt.
Because of the long catalyst residence time in the reactor, the size
of the regenerator is only l/2 of the size of the reactor Thus, the
use of the fluorine promoted catalyst enables a considerable reduction
in size of regenerator to be made as compared with that necessary when
using the non-promoted catalyst for fluid autofining.
If desired, the regeneration of the catalyst 7800 F.
Initial-100 p s i ga.
Equilibrium-500 p s i ga.
1.2 weight of oil/weight of catalyst/hour SCF/B (set at an initial
pressure of p s i ga) Spent catalyst was regenerated in a separate
reactor as follows 800 g of catalyst were charged to the reactor and
the temperature raised to 8000 F Cold air was injected at the base of
the reactor at a rate of 220 CF/hr /CF of catalyst This rate was
sufficient to fluidize the catalyst.
The burning temperature of the catalyst was controlled at 10500 F by
heat transfer through the reactor walls and minor adjustments of the
air rate When regeneration was completed at 8000 F, the reactor
temperature was raised to 10000 F, and the air treatment continued
until all carbon was removed.
Catalyst regenerated in this manner was found to have lost 0 2 % wt
fluorine When this catalyst was added to the autofining reactor,
tertiary butyl fluoride was dissolved in the gas oil feed in
sufficient quantity to deposit 0.2 % wt fluorine on the added
catalyst.
The autofining of a gas oil by the process of the present invention to
produce a gas oil of 0.1 % wt sulphur can be carried out on a
commercial scale under the following conditions.
Microspheroidal cobalt molybdate on alumina activated by the addition
of aluminium fluoride 1.0 weight of oil/weight of catalyst/hour 7800
F.
300 p s i ga (approximately) 3000 SCF/B (at 300 p s i ga) 250 hours
20.0 % 0.7 feet/sec.
may be carried out at atmospheric pressure 90 since the amount of
catalyst to be regenerated is small In this case, catalyst is
withdrawn either intermittecntly or continuously into a separate
chamber at atmospheric pressure where the catalyst is fluidized and
regenerated 95 ina stream of axygen-containing gases The regenerated
catalyst is then reduced and sulphided, using the gases ei-jclved

during the stabilization of the autofined products The pre-treated
catalyst is fed back into the unit by 100 means of a pressurized
hopper.
The advantages of this method of regeneration are:i The mechanical
difficulties of circulating and stripping the catalyst at high
pressures are 105 avoided.
ii It is possible to utilize the low pressure stabilizer gases for
pre-sulphiding and reduction of the catalyst.
The process according to the present inven 110 t tion may be carried
out commercially in a plant 785,312 as illustrated in the accompanying
diagram The oil to be desulphurised is passed vialine 10 and preheater
11 to a reactor 12 in which is maintained a fluidised bed of catalyst
as hereinbefore described The products from the reactor 12 pass via
line 13 to a high pressure separator 14 from which hydrogenrich
recycle gas is withdrawn via line 15 The product containing dissolved
hydrogen sulphide, light hydrocarbons and the remainder of the
hydrogen, is removed from the separator 14 via line 16 and passed to a
stabiliser for the removal of the dissolved gases The recycle gas
passes via line 15, preheater 17 and lines 18 to the reactor 12.
Catalyst is withdrawn from time to time into a stripper 19 from which
it passes via pipe 20 into a regenerator 21 Air is passed into the
regenerator 21 via line 22 and the regeneration gases leave via line
23 Excess heat is removed by means of a waste heat boiler 24
Regenerated catalyst is reurned to the reactor 12 via pipe 25 and
reducing zone 26 wherein it is treated with hydrogen which enters the
reducing zone from line 15.
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