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 described 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.


* GB785310 (A)

Description: GB785310 (A) ? 1957-10-23

Pipe couplings


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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. COMPLETE SPECIFICATION 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.


* GB785311 (A)

Description: GB785311 (A) ? 1957-10-23

Manufacture of combustible gas



DE1009344 (B) FR1136956 (A) DE1009344 (B) FR1136956 (A) less Translate this text into Tooltip



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.


* GB785312 (A)

Description: GB785312 (A) ? 1957-10-23

Improvements relating to hydrocatalytic desulphurisation processes



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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. Complete Specification Published Oct 23, 1957. Index at Accertance:-Classes 1 ( 1), AS(AIA: B 2 A: B 2 X); and 91, 02 C. International Classification: -a Olj Cl Og. COMPLETE SPECIFICATION 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. Complete Specification Published Oct 23, 1957. Index at Acceptance: -Csses 1 ( 1), A 3 (AIA: B 2 A: B 2 X); and 91, 02 C. International Classification: -301 j Clag. COMPLETE SPECIFICATION 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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