5596 5600.output

* GB786004 (A)

Description: GB786004 (A)

No title available

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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.

We, BADISCHE A Ni Li N & SODA-FABRIK AKTIENGESELLSCHAFT, a Joint Stock Company, organised under the laws of Germany, of Ludwigshafen on Rhein, Germany, 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:- For the preparation of calcium carbide from lime and coke according to the process, wherein coke is simultaneously burnt to supply the necessary reaction heat, and reacted with lime to form carbide, in a shaft furnace (hereinafter referred to as " the oxygen thermal process "), naturally larger amounts of coke are consumed than in the electro-thermal process in which the coke merely yields the carbon necessary for the reaction with the lime Since the coke contains considerable amounts of ash, which amount to about 10/ there is the risk in carrying out the oxygen-thermal process that the calcium carbide formed will be strongly diluted by fused ash While it is true that at sufficiently high temperatures the ash may be partly or almost wholly vaporised, the vaporised ash condenses in the colder parts of the charge which thereby become gradually enriched in ash to such an extent that finally ash remains in the calcium carbide and is withdrawn in the liquid form therewith.

We have now found that the enrichment of ash in the colder parts of the charge, i e. in the upper part of the shaft furnace, can be extensively avoided bv maintaining in the upper part of the shaft furnace a gas speed of at least 8 centimetres per second with reference to gas at O C and 760 torr and empty furnace space. lPrice 3 s 6 d l Besides the production of a high percentage calcium carbide (i e calcium carbide containing more than 80 % Ca C 2), the method of working according to this invention has the further advantage that the dreaded bridging of the shaft furnace is avoided because the condensed ash components are entrained by the gas sweeping through the charge and consequently it is impossible for bridges to form from charge material cemented together by condensed ash particles. The following example will further illustrate this invention but the invention is not limited to this Example. EXAMPLE. A shaft furnace for the production of calcium carbide according to the oxygenthermal process is supplied with such an amount of oxygen that the speed of the gas mixture formed by combustion of coke with oxygen and in the formation of carbide, consisting of about 97 % of carbon monoxide and about 3 % of carbon dioxide, hydrogen, nitrogen and oxygen, corresponds to 4 5 centimetres per second (with reference to 00 C and 760 torr and to empty furnace space) in the upper part of the shaft furnace. At this speed the furnace tends to bridge and the working of the furnace is very irregular The calcium carbide content of the melt drawn off fluctuates considerably and averaged over a period of continuous operation for 24 hours lies at only 6 Y 5 % of Ca C 2. By loading the same furnace having the same weight ratio of coke and limne in the charge with an amount of oxygen so much greater that the above-mentioned gas speed 786,004 PATENT SPECFICATION > l Date of Application and filing Complete Specification: Jan 10, 1956 No 786/56. Application made in Germany on Jan 14, 1955. Complete Specification Published: Nov 6, 1957. Index at Acceptance:-Class 1 ( 2), E 2 A 1. International Classification:-C Olb. COMPLETE SPECIFICATION. Improvements in the Production of Calcium Carbide by the Oxygen-Thermal Process. 786,004 amounts to 12 2 centimetres per second, bridging no longer takes place and the working of the furnace is very regular The carbide content of the melt drawn off lies on an average at 83 5 % Ca C 2 and

fluctuates only within moderate limits ( 81 2 to 86 7 %) over long periods By reducing the gas speed below 12 2 centimetres per second it is found that upon reaching a speed of 8 centimetres per second disturbances by bridging of the furnace just commence. This speed is therefore to be regarded as the minimum speed necessary.

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* GB786005 (A)

Description: GB786005 (A) ? 1957-11-06

Refractory bodies and method of making the same




PATENT SPECIFICATION Date of Application and filing Complete Specification: Jan 17, 1956 No 1545 /56. Application made in United States of America on Jan 28, 1955. Complete Specification Published: Nov 6, 1957. Index at Acceptance:-Classes 1 ( 2), E 2 A 2; 22, F( 1:7:12:16: 24: 33); and 87 ( 2), A 1 R( 34: 58), A 2 E 1 E. International Classification:-B 29 d, j C Oib CO 4 b. COMPLETE SPECIFICATION.

Reiractory Bodies and Method of Making the Same. We, THE CARBORUNDUM COMPANY, of Niagara Falls, in the County of Niagara and State of New York, United States of America, a Corporation organised and existing under the laws of the State of Delaware, United States of America, 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 new and improved bonded silicon carbide articles of manufacture and to a novel method for making them. Bonded silicon carbide bodies have been known and used for many years A number of different materials have been used to bond the grains or Darticles of silicon carbide together to form the desired shape, such as clays and glass-forming mixtures of various composition to form conventional ceramic and vitreous bonded shapes, pitch and other tarry matter to form coke-residue bonded bodies, and more recently, silicon and silicon alloys fired under proper conditions so as to react with constituents of the ambient atmosphere to form refractory nitride and/or carbide bonds The bonded silicon carbide bodies obtained with these various prior art bonding compositions and methods have been satisfactorily used for many purposes, especially in the refractory field However, regardless of the type of product heretofore provided, each specific one has had its own particular disadvantages and limitations of use For example, the coke-residue bonded articles have been unduly susceptible to oxidation at elevated temperatures, and the vitreous-bonded and clay-bonded articles have shown a tendency at higher temperatures to soften and lose their strength with loss of desirable loadbearing ability Those silicon carbide bodies bonded by means of silicon nitride 45 and silicon carbide derived from silicon or silicon alloys have been shown to have exceptionally high strengths at high temperatures and also good load-bearing properties at elevated temperatures However, such 5 o bodies in certain applications wherein they have been subjected to severe or rapid fluctuations of temperature have not been entirely satisfactory and have failed due to cracking from heat shock 55 Furthermore, the moulding techniques employed in the making of bonded silicon carbide bodies, and particularly those of complex or intricate shape, have been subject to various limitations For instance, 60 while the clay-containing mixes due to the plastic nature of the bond constituents, lend themselves fairly well to the formation of shapes by the conventional methods of slipcasting from thin slip-casting slurries, the 65 resulting bodies do not have the requisite properties for some high temperature service conditions In fact, such bodies when made by normal slip-casting operations have been inferior to bodies of the same composition 70

formed by pressure moulding On the other hand, the more refractory bodies composed of non-plastic bonding constituents, such as those derived from silicon and silicon alloys, are not adaptable to normal slip-casting 75 operations and as a result the manufacture of such bonded bodies has heretofore been restricted to the simpler shapes which can be fabricated by conventional pressure moulding 80 It is an object of the present invention to provide a new bonded silicon carbide body having improved properties. It is a further object to provide bonded p A 786,005 silicon carbide articles having high resistance to heat shock. It is a still further object to provide a novel method of making bonded silicon carbide bodies having uniform body structure and improved properties, and particularly bodies of intricate or complex shape, from non-plastic compositions of the aforesaid type. According to the present invention a method of making bonded silicon carbide articles of manufacture comprises preparing an intimate raw batch mixture comprising granular silicon carbide, and a silicon-based material such as silicon or a silicon alloy, moistening said raw batch mixture with further mixing to bring it to the consistency of a sluggish mass, preferably ageing the mass, feeding raw batch of material into a wet plaster-graphite mould while subjected to mechanical vibration, drying said mould and contents, and firing the moulded article in a non-oxidizing atmosphere containing nitrogenous or carbonaceous or nitrogenous and carbonaceous constituents Usually a small amount of a temporary binder and/or a deflocculant is added The mass may be aged, preferably in a convered container, for a period of two to eight days prior to use. The aged mass may then be fed into a wet graphite-plaster of paris mould while the mix and the mould are simultaneously subjected to mechanical vibration which brings about a flow of the mix into the outermost corners and cavities of the mould and compacts the material to a dense, uniform structure The mould and contents, after a suitable period of agitation by mechanical vibration, are placed in a drying oven and the mould and contents dried Preferably the moulded article is still supported by all or part of the mould during firing In order to further assure that the atmosphere will be fully ncnl-oxidizing in character during the firing step, the usual practice is to surround the shapes while they are being fired with a carbonaceous packing material such as a mixture of fine graphite and coarse fragments or pieces of graphite During the firing of the articles the mould, when it is used to support the article during firing, gradually disintegrates to the extent that it is readily separated from the fired article at the conclusion of the firing process although it holds together during the firing process sufficiently to provide a

satisfactory support for the article during most of the firing process It is also noted that the cast article in the course of firing does not undergo perceptible change in size by either expansion or shrinkage so that as a result the article can be cast to certain desired final dimensions directly with the maintenance of unusually close dimensional tolerances. The firing may take place in a nonoxidising nitrogenous atmosphere such as an atmosphere of nitrogen or ammonia Alternatively the moulded articles can be fired in a non-oxidising, carbonaceous atmosphere such as an atmosphere of carbon monoxide, or in a non-oxidizing atmosphere containing both nitrogenous and carbonaceous components whereupon the carbon oxide gases of the ambient atmosphere, or the carbon oxide gases and nitrogen together of the ambient atmosphere, react with the silicon and/or silicon alloy of the bond to form an ultimate interstitial bond of silicon carbide or silicon carbide and silicon nitride in combination, depending upon the absence or presence of nitrogen or nitrogen-yielding constituents in the atmosphere The silicon carbide thusly formed within the body of the article is of the cubic crystalline habit and, with or without the silicon nitride as the case may be, forms an interstitial bonding matrix for the granular silicon carbide constituting the major component of the body. PREPARATION OF SLUDGE-CASTING MIX Mix No 1. Silicon carbide, mesh and finer Silicon carbide fines Ferromanganese silicon, mesh Silicon, 200 mesh Bentonite Water Dextrine Lithium citrate, ' aqueous solution Mix No 2. Silicon carbide, mesh and finer Silicon carbide fines Silicon, 200 mesh Bentonite Water Dextrine Lithium citrate, % aqueous solution so lb. lb. 101 b. l Olb. O 5 lb. 4800 cc. 0 24 lb. 520 cc. lb. l Olb. 151 b. 0 5 lb. 4800 cc. 0 24 lb. 520 cc. Using either one of the two mixes set forth above, all the ingredients except the water and lithium citrate are mixed dry to form an intimate

mixture after which the 115 water and lithium citrate are added, either separately or together, and mixed for approximately ten minutes The resulting wet mix is then left in the mixer or transferred to a container and covered over with 120 a wet burlap bag or otherwise protected against undue evaporation of water from the mix and allowed to age for between two and eight days before use It has been found that where such mixes have been 125 allowed to stand for several days and the 786,005 forms as a temporary binder to give the body sufficient "green" strength for handling before firing Other deflocculants and/or temporary binders that are well known in the trade can be similarly used, or the deflocculant and/or temporary binder can be eliminated without departing from the scope of the present invention For example although it is usually desirable to use a small amount of a temporary binder to lend handling strength to the unfired body, such temporary binder can be dispensed with in some cases such as when the formed article is to be fired prior to its removal from the mould. MOULDS. The moulds used for carrying out the present process are made of a combination of plaster and graphite with or without the use of other filler materials such as sand, crushed mould residue, or walnut shells. The graphite content of the mould mix has been found to be advantageous to the release of the mould from the cast article, separation being much easier than in the case of straight plaster moulds where it would be practically impossible to satisfactorily separate the two Satisfactory moulds and cores have been made from the following compositions:mix allowed to lose too much of its moisture it will not satisfactorily cast and it must be reconditioned by the addition of water to re-wet the mix, followed by remixing. The sludge-casting mix should always be aged to get the maximum density and uniformaity of body structure in the formed article, as is customarily desired for most purposes However, for the few occasions whler it is not essential to provide optimum density in the finished piece and a more porous, permeable structure can be tolerated for the use in mind, it has been found that the ageing step can be eliminated and the unaged mix cast and ruleased from the mould, although the resulting body is less dense and has a more porous and more permeable appearance. It is not desired to be limited to the specific mixes set forth above since satisfactory results have been obtained using finer grit size silicon carbide than the 10 mesh and finer material specified in the above mixes. It is also possible to use other proportions of ingredients without

departing from the scope of the invention. In the two specific mixes set forth above, the lithium citrate acts as a deflocculating agent and the dextrine serves not only as an added deflocculant but to some extent perMould Mix No. Mould Ingredients 1 2 3 4 % by % by % by % by Weight Weight Weight Weight Pottery plaster 50 67 S 5 67 Powdered graphite 50 33 25 15 Sand 20 10 Walnut shells 5 8 The amount of water may vary somewhat cast article does not have a homogeneous with different grades of plaster, but it should structure Actually, if the mould is made be somewhere in the neighbourhood of 50 % and allowed to stand any substantial period 95 water and 50 % plaster and graphite mixture of time prior to use such as longer than one by weight The correct amount of water day it should be re-wet in order to paris placed in the container and the plaster tially fill the pores with moisture prior to and graphite mixture is sprinkled in gradu use. ally until all the dry mix has been added. The mixture is then mixed with a high SLUDGE-CASTING TECHNIQUE 100 speed mixer for a very short period of time The properly aged mix is placed on a such as a half minute The mixture is then vibrator and vibrated for approximately 4immediately cast around the pattern or hour immediately before using While the model to form the desired mould The mix is being vibrated it should be continumodel is first coated with a parting medium ally turned over and mixed with a trowel 105 such as a Special Oil soap solution available This is done to render the mix completely under the trade name "Vos XX" or a paste homogeneous and also serves as a means of wax in order to provide a means of separ determining whether the mix has been suffiation of the mould from the pattern after ciently aged If free water forms upon the setting The moulds are ready for use as top of the mix during this preliminary vibra 110 soon as the plaster has set u D since the ting stage it is an indication that the mix moisture contained in the mould body serves is not homogeneous and should be further to prevent an excessively rapid extraction of aged before casting Although the casting moisture from the cast body when the mould mix is invariably of a heavy, sluggish sludgeis used When the water is withdrawn from like nature the consistency of the casting 115 the mould contents too rapidly the resulting body can vary to some extent depending 786,005 upon the particular shape to be cast For instance, thicker sections can use a much stiffer mix than the thinner-walled more intricate shapes However, in no case should the mix be used if it is found to have free water on the surface of the mix as a result of the preliminary vibrating operation. The wet plaster-graphite moulds are either clamped or held together by rubber bands and placed on the vibrating table and the mix fed into

the mould cavities by means of a filling chute The filling chute is rested upon a block or other support that will transmit vibrations to the mix passing from the chute to the moulds Very satisfactory results have been obtained by placing the entire mix container on the vibrating table during the filling of the mould so that the entire mass is subjected to constant vibration so as to keep the material agitated and conditioned for use, but a vibrating feeder is usually found preferable It might be noted that the casting mass is of sufficient stiffness or sluggishness that it does not flow until subjected to some form of vigorous agitation or mechanical vibration. After the mould is completely filled with a slight surplus to allow for shrinkage the mould is left on the vibrator and allowed to vibrate at a lower frequency for a short period of time in order to further compact the mould contents During this period, small increments of additional casting mix can be added at the entrance to the mould cavity in order to fill voids and replace any water absorbed by the mould When no more material will go into the mould the top can be struck off with a trowel and the mould placed in a drier and dried at 1400 F overnight After drying, the mould can be removed from the cast shape if desired. This is done by tapping the mould lightly just enough to break the contact between the mould and the piece However, most satisfactory results are obtained by leaving the mould on the cast shape or at least a part of the mould on the cast shape to provide support and placing both in the kiln for firing. FIRING OPERATION. The cast article supported by at least a part of the mould structure, is placed in a suitable kiln or furnace chamber and fired in a non-oxidising nitrogenous atmosphere at a temperature of 14000 C to 1450 C, the furnace being held at peak temperature for a period of several hours in order to allow time for completion of the reaction between the nitrogen introduced and the silicon and/or silicon alloy to form a silicon nitride or silicon nitride containing bond for the silicon carbide particles The temperature limits may be above and below those indicated It has been found desirable to surround the articles in the kiln or 63. furnace chamber with a sufficient amount of carbon to take up any oxygen which might otherwise serve to react with the cast piece during firing. As already pointed out, instead of firing the 7 " moulded and dried shape in an atmosphere of nitrogen or in a nitrogen-generating atmosphere such as an atmosphere of ammonia, the article can be fired in a non-oxidising. carbonaceous atmosphere, such as an 73 atmosphere of carbon monoxide

whereupon the carbon oxide reacts with the silicon andlor silicon alloy bonding components to form a silicon carbide of cubic crystalline habit which serves to bond the granular So silicon carbide of the body together. As has been herein described, the granular silicon carbide of the articles is held together by a bond of silicon nitride andlor silicon carbide, depending upon the specific 85 character of the non-oxidizing ambient atmosphere within the firing chamber and the conditions of the firing step Generically speaking, these various bonding ingredients, namely, silicon carbide and silicon nitride, 9 ba can be otherwise referred to as silicides of carbon and nitrogen, or, in other words, as non-metallic silicides. The resulting sludge-cast silicon carbide articles are characterized by having an 95 extremely smooth, dense surface appearance characteristic of articles formed by wet casting and also have extremely uniform, dense body structures throughout Sludgecast silicon carbide articles of the herein 100described type are also highly resistant to fracture when subjected to extreme fluctuations in temperature This resistance to breakage by heat shock is an entirely unexpected property which contributes greatly 105 to the value of the material for certain high temperature applications where extreme fluctuations of temperature are encountered. The material also has a bell-like ring when struck with a Diece of metal Since 110 the overall density of the cast bodies is usually slightly lower than pressed bodies of similar composition, this soundness of body is believed to be due to the extremely uniform density throughout the niece and is res 115 ponsible at least in part for the high heat shock resistance In several tests where articles of the present invention have been compared directly with otherwise moulded or pressed shapes of similar composition it 12 C 1 has been shown repeatedly that the heat shock resistance of the present bodies is anywhere from two to three times as good as shapes made by conventional prior art methods This comparison is based on the 12 ' number of cycles to which the two different materials can be exposed to extreme heat shock before cracking appears. The herein-described process has extended 786,005 silicon alloy, moistening said raw batch mixture with further mixing to bring it to the consistency of a sluggish mass, prefer 55 ably ageing the mass, feeding the raw batch of material into a wet plaster-graphite mould while subjected to mechanical vibration, drying said mould and contents, and firing the moulded article in a nonsoxidizing 60 atmosphere containing nitrogenous or carbonaceous or nitrogenous and carbonaceous constituents.


* GB786006 (A)

Description: GB786006 (A) ? 1957-11-06

Primary aliphatic amines and/or their hydrohalides and process of producingthe same

Description of GB786006 (A)

COLBTE SiPECIIFIGATIOiN Primary Aliphatic Arnines and/or their Hydrohalides and Process of producing the same We, OLIN MATHIESON CHEMICAL SCOR PORATION, a corporation organised under the laws of the State of Virginia, 'United States of America, of Ten Light Street, Baltimore 3, Maryland, United States of America, 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 a process for the manufacture of primary aliphatic amines. in which the formation of undesirable by-pro ducts is substantially suppressed and which is particularly useful in the manufacture of ethylene diamine. The reaction of suitably reactive organic halides with ammonia to form the corresponding primary amines is well knows and has been widely investigated. The reaction, although a simple one, is complicated by the formation of various undesirable by-products such as secondary amines, tertiary amines and quaternary ammonium compounds. It has been found that the formation of these undesirable byproducts can be at least partially suppressed by employing an excess of ammonia in the reaction. This knowledge has

not, however, provided the art with an entirely satisfactory solution to the problem of suppressing the formation of non-primary amine by-products due to the high vapor pressure of ammonia which has necessitated conducting the reaction in pressure vessels with resultant increased production costs. This dlifficulty has also been partially overcome by using water to reduce the vapor pressure of ammonia. Although methods employing water and elevated pressures have been partially .successful in suppressing the formation of non-primary amine bywproducts, it has still been necessary to strike an economic balance between the costs of recovering and recycling large volumes of a3xmon.ia and the alternative of producing less primary amine and more of the und!esir- able secondary and tertiary amines. The choice between these economically unattractive alternatives has previously been unavoidable. As a general rule the ratio of ammonia to organic halide has been sufficiently low to avoid excessive recycle costs and yet high enough to produce adequate yields of primary amine without the formation of excessive amounts of the less valuable by-products. In the production of ethylene diamine, for example, a ratio of ammonia to organic chloride of from 5:1 to 15:1 has been commonly employed according to lGroggins, "Unit Processes in Organic Syntheses." These ratios of ammonia to organic chloride, although as high as generally practicable in imown processes, result in the formation of relatively large quantities of undesirable biy-products having a lower economic value than ethylene diamine, e.g. diethylene triamine, triethylene tetramine and higher polyethylene polyamines. The present invention provides a method for the production of primary aliphatic amines in which the formation of undesirable by-product amine compounds is substantially suppressed due to the maintenance of a very high ratio of ammonia to aliphatic halide in the reaction zone. The present invention, although widely applicable in the preparation of primary aliphatic amines, is particularly useful in the preparation of ethylene diamine and provides a method for producing this compound 'with substantially no production. of the undesirable polyethylene polyamines. This desirable result is accomplished while maintaining the cost of recycling ammonia within reasonable limits.. According to the invention, there is provided a process for the production of primary aliphatic amines and their hydrohalides, which comprises reacting an aliphatic halide which forms a water azeotrope boiling in the range extending from the boiling point of ammonia to the boiling point lof water with ammonia in the central portion of a vertical reaction zone, charging water to said zone or a point above the central portion thereof whereby the resulting primary aliphatic

amine hydrohalide is dissolved and. removed as an aqueous solution from the central portion to the lower portion of said zone, distilling dissolved reactant ammonia and aliphatic halide from said aqueous solution in the lower portion of said zone to return said reactants to the central portion of said zone, refluxing ammonia in. the upper portion of said zone, and recovering an aqueous primary aliphatic amine hydrohalide solution from the lower portion of said zone, and if desired, neutralizing the primary aliphatic amine hydrohalide to obtain the corresponding free amine. In carrying out the process of the present invention, a suitable aliphatic halide, water and ammonia are charged to a vertical reaction zone which in practice can be a conventional fractionating tower. The reaction zone is maintained under suitable conditions of pressure and temperature to condense substantially all of the excess ammonia passing overhead with the result that the ammonia is returned totally as reflux to the upper portion of the reaction zone or, optionally, the ammonia can be recycled to lower portions of the zone as well. The reaction of the aliphatic halide with ammonia occurs in the central portion of the reaction zone or fractionating tower. The effluent from the lower portion of the reaction zone comprises an aqueous solution of the primary amine product, usually in the form of its hydrohalide salt Suitable temperatures are maintained in the lower portion of the reaction zone to free the aqueous solution present at that point from excess ammonia and aliphatic halide, thus retuming the reactants to the central portion of the reaction zone or fractionating tower and providing an aqueous product containing effluent free from dissolved reactants. Since ammonia is always the most volatile substance in the system, it is possible to retain the aliphatic halide reactant in the central portion of the reaction zone by refluxing ammonia in the upper portion of the zone. Therefore by maintaining suitable tern- peratures in the upper and lower portions of the reaction zone, the reactants are concentrated in the central portion of the zone, making it possible to maintain at that point a very high ratio of ammonia to aliphatic halide. This effectively suppresses the formation of the undesirable by-products referred to above, thus providing for the production of a primary aliphatic amine in an economical and efficient manner. The process can be operated in a batch or continuous manner. When operated continuously, the ratio of make-up ammonia to aliphatic halide charged to the tower may be substantially theoretical once the unit is in operation. The fresh charge is chemically equivalent to the amount of primary amine product removed from the lower portion of the reaction zone or fractionating tower, e.g., when one pound-mole per minute of ethylene diamine dihydrochloride is removed as an aqueous

solution from the lower portion of the reaction zone, one pound-mole of ethylene dichloride and two pound moles of ammonia per minute are charged as make-up to the reaction zone. The superiority of the present process to those of the prior art is obvious when it is considered that reaction of stoichiometric proportions of aliphatic halide and ammonia would ordinarily produce substantial amounts of the undesirable by-products and commercially inadequate yields of the desired primary amine. For example, when ethylene dichloride and ammonia are reacted in theoretical proportions, polyethylene p olyamines are formed as principal products and relatively little of the desired product, ethylene diamine, is obtained. In the present process, however, due to the fractionation which takes place in the reaction zone, the reaction occurs in the presence of an extremely high ratio of ammonia to ethylene dichloride and, therefore, satisfactory yields of ethylene diamine are obtained with substantially no formation of polyethylene polyamines. The heat of reaction is usually sufficient to maintain an adequate reaction temperature in the central portion of the reaction zone so that no additional heat is ordinarily required at this point Any excess heat which is generated by the reaction may be removed by cooling and condensing the ammonia overhead and refluxing or recycling the cooled ammonia to the reaction zone. If necessary, heat may be supplied to the lower portion of the reaction zone or fractionating column or to a separate stripper section to insure the removal of dissolved aliphatic halide and ammonia from the effluent aqueous product-bearing solution. Water is charged to the reaction zone in an amount sufficient to maintain all of the reaction product in aqueous solution. Suitable holding times are automatically provided in the present method by controlling the product take-off rate and the reactant charge rate. The temperatures and pressures which are suitable for use in the present process vary, depending upon the aliphatic halide employed! in the reaction. Ordinarily, temperatures of about 30 to 40 C. in the upper portion of the reaction zone or fractionating tower and from about 100 to 2009 C. in the lower portion of the reaction zone are suitable. Suitable pressures include those from about atmospheric to about 300 pounds per square inch or more. In a modification of the present process, part of the water charged to the reaction zone may carry with it a suitable proportion of a water-soluble non-volatile alkali provided that the alkali is charged to the reaction zone at apoint below that at which appreciable quantities of aliphatic halide are present. Although any water-soluble non-volatile alkali may be used, sodium hydroxide is preferred because

of its low cost and ready availability. Some water is ordinarily charged to the reaction zone at a higher point in order to depress the vapor pressure of ammonia and insure the solution of the primary amine hydrohalide product. Charging the aqueous alkali to the reaction zone or fractionating tower at a point below that at which substantial amounts of aliphatic halide are present avoids hydrolysis of the aliphatic halide and converts the primary amine hydrohalide product and any ammonium halide present to the free amine or ammonia and alkali halide. The relatively vol tile ammonia thus liberated is returned to the central portion of the reaction zone as described above. Water and sodium chloride are of much lower volatility than any of the other substances present in the system described above and are, therefore, easily removed from the lower portion of the reaction zone as an aqueous solution. The introduction of alkali produces additional heat in the reaction zone and liberates this heat at a point of maximum usefuLness. In the modification of the present process in which no alkali is introduced into the reaction zone, the effluent aqueous solution contains the primary amine hydrohalide which may be neutralized separately. This method wastes the heat of neutralization. The primary amine product may be removed from the aqueous salt solution, obtained as. described above, as an azeotrope with water or as the anhydirous amine by conventional methods. The process of the present invention is useful for the ammoniation of aliphatic halides where the 'water azeotrope of the halide to be converted has a boiling point above that of ammonia (-33 C. at standard conditions) and below the boiling point of water. In the modification of the present invention in which a water-soluble non-volatile alkali is employed, suitable aliphatic halides are those which form water azeotropes distilling at temperatures below that at which the water azeotrope of the primary amine corresponding to the halide has a substantial vapor pressure. In other words, alkali may be used only with aliphatic halides whose water azeotropes have relatively low boiling points, whereas in the modification of the present invention in which no alkali is employed, aliphatic halides which form water azeotropes boiling at relatively high temperatures but still below the boiling point of 'water may be used since the product is obtained in the form of the relatively less volatile primary aliphatic amine hydrohalide. In general, then, it is necessary to seleot aliphatic halide reactants which can be volatilized from an aqueous

solution containing the product without volatilizing significant amounts of the product. The product is removed from the central portion of the reaction zone immediately after formation as an aqueous solution which is then subjected, in the lower portion of the reaction zone, to a temperature sufficiently high to remove dissolved aliphatic halide from the solution. In this way, contact of product and reactants is kept to a minimum and the formation of undesirable by-products such as secondary and tertiary amines is minimized^. Aliphatic halides which are suitable for use in the modification of the process of this invention in which a water-soluble non-volatile alkali is employer to obtain an aqueous primary aliphatic amine solution as a bottoms product include methyl chloride, ethyl chloride, and ethylene dichloride. The water azeotropes of the aliphatic halides of this category have boiling points which are sufficientiy lower than those of the water azeotropes of the corresponding primary amines to make separation of the reactant halide from the aqueous pro duct-b earing solution relatively easy. Temperatures in the reaction zone are generally low so that longer reaction times are ordinarily required for these volatile halides. Certain higher boiling aliphatic halides may also be used when alkalies are employed. These include, for example, propylene dichloride and n-butyl chloride. The former boils at 96.8 C. at atmospheric pressure but steam-distills from an aqueous solution substantially completely while propylene diamine, which boils at 120 C., is largely retained in the aqueous solution. In like manner, n-lbutyl chloride and n-butyl amine boils tat 77.5 C. and 77" C., respectively, but the former is readily volatilized with water vapor while the n-butyl amine has a relatively low vapor pressure in aqueous solution. Certain other aliphatic halides 'which are useful in the process of the present invention have boiling points which; are too high to allow the use of alkali. These halides which include trimethylene chloride, ethyl bromide, methyl halide, and cyclopropylr chloride may be steam-distilled from an aqueous solution containing the corresponding primary amine hydrohalide and are, therefore, useful in the modification of the present invention in which no alkali iis employed. By contrast, halogen atoms attached directly to aromatic nuclei are usually too unreactive to make the preparation of primary aromatic amines feasible by the method ,of this invention. Further, aromatic compounds containing ,halogen atoms sufficiently reactive because of their position in aliphatic side chains or due to the presence of activating nuclear substituents are also unsuitable since these compounds are usually too high boiling for use in an aqueous system. On the other band, although most fluorocarbons are insufficiently

reactive for conversion by the present process, such compounds containing a more reactive haLogen atom may be used with advantage. For example, 2,2,2,-trilquoro-I-chloroethane yields 2,2,2 -trifluoro-ethylamine. The invention will be further illustrated by reference to the attached drawing. Ethylene bichloride water and ammonia are introduced by lines 11, 12 and 13 respectively to fractionating tower 14, which may be of the bubble cap lor packed type. Recycle ammonia, if used; is also introduced to the tower at one or many points by line 15. The heat of reaction generated in the tower serves to evaporate ammonia and ethylene dichloride which are fractionated, ammonia passing overheady via line 16 and ethylene dichloride remaining in the mid-portion of the tower. Ammonia is liquefied in cooler 17 and either totally or partly returned to the tower as reflux by line 18. The remaining ammonia flows through line 19, controlled by valve 20, to surge tank 21 and is recycled to the tower via line 15. The ratio of ammonia used for reflux and for recycle is controlled by valve 20. Water and ethylene diamine dihydrochloride pass downwardly in the tower, vaporizing ethylene dichloride therefrom and returning it to the mid-portion of the tower. The bottoms, free of ammonia and ethylene dichloride, are removed through line 22 and in part pass by line 23 to reboiler 24, returning vapors by line 25 to the bottom of the tower. The product, ethylene diamine dihydro- choride in aqueous solution, is removed by line 25. In the alternative procedure in which the base is liberated by means of caustic soda, the latter may be charged in aqueous solution t a line 27 entering the tower 14 at a point below the inlet line 13 for make-up ammonia. The bottoms product then comprises an aqueous solution of sodium chloride and ethylene diamine, from which the latter may be recovered in any lonown manner. The invention will be further illustrated by reference to the following example: In an operation similar to that shown in the attached figure, with the exception that the inlet lines to withe tower are modified by vertical adjustment thereof and in which the tower is about 35 feet in height and 0.25 square foot in cross-sectional area, 100 pounds per hour of ethylene dichloride are charged through a line entering the fractionating tower just below the top plate. Fresh anhydrous ammonia enters the tower at the rate of 35 pounds per hour through a line located about one third of the distance above the bottom of the fractionating tower. A line located about one-fifth ,of the height of

the column from the bottom carries 200 pounds per hour of 40% caustic soda. A line located at about the level of- the second plate from the top of the fractionating tower carries 315 pounds per hour of additional water. Heat is supplied by the reaction of the ethylene dichloride, ammonia and caustic soda in the fractionating tower, and additional heat is introduced in the reboiler. The liquid and vapor in equilibrium on the top plate are substantially anhydrous ammonia. Under a pressure of 225 psig, ammonia gas is removed from the top of the tower at about 38 C. It is taken overhead at a rate of about 568 pounds per hour to the cooler, which reduces the temperature of the liquid ammonia to about 35 C. About half of the ammonia is returned to the top plate of the tower as reflux, and about half is returned through a surge tank to the reacrion zone of the tower at about the mid-point thereof. The ratio of ammonia to ethylene dichloride is about 33 1. The liquid level in the bottom of the tower is just sufficient to maintain liquid feed to the reboiler. The bottoms leave the tower at a temperature of about 140 C. and comprise an aqueous solution of about 9% of ethylene diamine and 18 of sodium chloride. Ethylene diamine can be separated therefrom by distillation or other suitable means. What we claim is: - 1. A process for the production of primary aliphatic amines and their hydrohalides which comprises reacting an aliphatic halide which fonms a water azeotrope boiling in the range extending from the boiling point of ammonia to the boiling point of water with ammonia in the central portion of a vertical reaction zone, charging water to said zone at a point above the central portion thereof whereby the resulting primary aliphatic amine hydrohalide is dissolved and removed as an aqueous solution from the central portion to the lower portion of said zone, distilling dissolved reactaut ammonia and aliphatic halide from said aqueous solution in the lower portion of said zone to return said reactants to the central portion of said zone, refluxing ammonia in the upper portion of said zone, and recovering an aqueous primary aliphatic amine hydrohalide solution from the lower portion of said zone, and if desired neutralizing the primary aliphatic amine hydrohalide to obtain the corresponding free amine. 2. A modification of the process according to claim 1, in which the water azeotrope of said aliphatic halide has a boiling point which is less than the 'boiling point of the water azeotrope of the primary aliphatic amine corresponding to said aliphatic halide, which includes charging a water-soluble non-volatile alkali to the reaction zone below the central portion of said zone at a point where said alkali will not come in contact with substantial concentrations of the reactants to convert said primary aliphatic amine hydrohalide in said

aqueous solution in the lower portion of said zone to the free amine, and recovering an aqueous primary aliphatic amine solution from the lower portion of said zone. 3. A process according to claim 2, in which the water-solubIe non-volatile alkali is sodium

* GB786007 (A)

Description: GB786007 (A) ? 1957-11-06

Thiazolo-pyrimidines




PATENT SPECIFICATION 786 0007 Date of Application and filing Complete Specification: Jan 30, 1956. No 2950/56. Complete Specification Published: Nov 6, 1957. Index at acceptance:-Class 2 ( 3), C 2 A( 3: 14), C 2 C( 4: 6 B: 7 A 1), C 2 R( 15: 18). International Classification:-CO 7 d. COMPLETE SPECIFICATION Thiazolo-Pyrimidines We, THE WELLCOME FOUNDATION, LIMITED, a British Company of 183-193 Euston Road, London, N W 1 do hereby declare the;invention (Communicated by Burroughs Wellcome & Co (U S A) Inc, of Scarsdale Road, Tuckahoe 7, New York, in the county of Westchester, State of New York, United States of America, a Corporation organised under the laws of the State of New York, United States of America) 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 present invention relates to new derivatives of pyrimidine namely thiazolo ( 5,4-d) pyrimidines and the method of preparing the same. Thiazolo ( 5,4-d) pyrimidines are of interest because of the structural analogy to the imidazolo ( 5,4-d) pyrimidines (purines). Earlier attempts to, prepare the analogues of the natural purines gave examples with additional substituents (e g 2-phenyl, 2-methyl, see Falco and Hitchings, J Am Chem Soc 72 3203 ( 1950)) but the methods then employed failed to provide the substances with hydrogen in the 2-position The thiazolo ( 5,4-d) pynimidines are of interest as a new series of biologically active materials useful against lactic acid bacteria and having properties which render them, of interest in the treatment of neoplastic growth including human leukemias. The compounds which are the subject of the present invention are 7-aminothiazolo ( 5,4-d) pyrimidine and 5,7-diaminothiazolo ( 5,4-d) pyrimidine, and may be represented by the formula (I), (I) wherein R is amino or hydrogen It has been found that these compounds may be readily prepared by a reaction involving the treatment of 4,5-diamino-6-mercaptopyrimidine or 2,4,5triamino-6-mercaptopyrimidine (II) with concentrated formic acid. This method may be illustrated as follows: SH A (IH ( 1 I) S CH H-c CO Nc ENTRATED H Co 2 H (I) The following examples illustrate the methods employed herein and the recovery of the desired compounds. EXAMPLE I. 4,5-Diamino-6-Mercaptopyrimidine. 7.5 Grams of 4-amino-6-chloro-5-nitropyrimidine was suspended in 200 ml of 1 Apotassium hydrosulphide and heated on the isteam bath for two hours while passing hydrogen sulphide through the reaction mixture. The reaction mixture was allowed to cool slowly, acidified with 10 N sulphuric acid and chilled The precipitate consisted of 4,5-diamino-6-mercaptopyrimidine and sulphur It was boiled with 300 ml of water, filtered hot and then chilled The product precipitated as pale yellow needles ( 4 2 g); an additional 0 95 g was obtained by concentration of the mother liquors to 100 ml The ultraviolet absorptionl spectrum of 4,5-diamino-6-mercaptcpyrimidine shows maxima at 240 and 305 my A at p H 1 and at 240 and 310 my at p 11 11. 7-Amino-thiazoleo ( 5,4-d)-pyrimidine. -A mixture of 2 g of 4,5-diamino-6mercaptopyrimidine and 10 ml of 98 % formic acid was heated at 70 for two hours and thenl evaporated to dryness on the steam bath The residue, 7-amino-thiazolo ( 5,4-d) pyrimidinc has an ultraviolet absorption spectrum completely different from the starting material Amax -263 mp A at p H 1; Amax -261 mat at p

H 11. EXAMPLE II. 7-Aminothiazolo ( 5,4-d) pyrimidine. 9 g of 4,5-diamino-6-mercaptopyrimidine was allowed to stand with 100 ml of 98 % formic acid for 2 days at room temperature. The mixture was evaporated to dryness on the steam bath and the residue recrystallized from ml of water, adjusted to p H 7 with ammonium hydroxide On cooling, colorless needles of 7-aminothiazolo ( 5,4-d) pyrimidine precipitated, m p 2140 (yield = 7 1 g-) The ultraviolet absorption spectrum shows a single band with Amax = 263 mpl at p H 1 and p H 11. EXAMPLE III. 5,7-Diaminothiazolo ( 5,4-d) pyrimidine. 0.5 g of 2,4,5-triaminn-6-mercaptopyrimidine was heated with 30 ml of 98 % formic acid at 1000 for five hours and the solution was then evaporated to dryness on the steam bath The residue was suspended in 50 ml of water and the p H adjusted to 8 with ammonium hydroxide The insoluble material was removed by filtration The 5,7-diaminothiazolo ( 5,4-d) pyrimidine was obtained by evaporation of the aqueous filtrate to dryness, and extraction of the residue with 50 ml. of ethyl alcohol Evaporation of the alcoholic solution gave 5,7-diaminothiazolo ( 5,4-d) pyrimidine which shows the following ultraviolet absorption spectrum: Amax = 265 ma. at p H 1 and Amax = 285 m at p H 11.


* GB786008 (A)

Description: GB786008 (A) ? 1957-11-06

Conveyor apparatus for the evacuation of dusty or grain material frompressure tanks by means of compressed air

Description of GB786008 (A)

COMPLETE SPECIFICATION Conveyor Apparatus for the Evacuation of Dusty or Grain Material frozen Pressure Tanks by means of Compressed Air I, MAX RINGER, a German Citizen, of 70, Wiesbadener Strasse, Dotzheim-Wiesbaden, Germany, trading as KLINGER K. 'G., do hereby declare the invention, for which 6 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 sttement: - This invention relates to pneumatic conveyor apparatus for rransporting dusty or fine gained materials ;such as cement. More particularly, it relates to the ,construction of a nozzle member adapted to be used in pneumatic apparatus for the vertical conveyance of fine grained material the term " vertical conveyance " being used in the sense that the material to be conveyed is drawn up through the nozzle member ;iito the conveyor standpipe, and ,thence outside the container holding the material, as distinct from conveyance downward by means of discharge jackets or nozzles mounted on the container. As is well known, containers of various design are used for transporting dusty or fine grained materials such as cement. These containers may normally be held in upright positions, rounded at the bottom or tapering downward in a cone, and it is of course common for them to be mounted on vehicles. The containers may also be placed horizontally and he cylindrical or pear-shaped, or they can be rectangular with rounded edges. fFor transferring the material from these tanks to other fixed containers various pneu- mastic conveyor devices can be used. Two basic methods are knows for accomplishing this purpose, the first being conveyance downwards fnom so-called discharge jackets or nozzles mounted on the container, and the second being "vertical conveyance" wherein the material inside the tank is forced upwards, ;by means of air pressure or the like, through the nozzle and into la conveyor stand-pipe. In each case the material must first be loosened and this is effected Iby blowing air up into the material through some type of air inlet device mounted on the bottom side of the tank. ,Except in the case of upright, conical containers, the material must then be transported to the discharge jacket or nozzle. In hrnzon- tal beilers, for example, fittings iare installed at a given angle for the purpose of itranspont- ing the material with or without the aid of air, depending on the slope, to these discharge jackets. The proper

inclination of the tank can also be obtained by tipping it. Experience has shown that the pneumatic ,oonveyance of dusty materials wherein the material is forced downwards through discharge jackets or nozzles at the lowest point of the tank 'consumes a greater amount of energy and is therefore less efficient than vertical conveyance methods wherein the material is forced upwards through the nozzle into the conveyor stand-pipe. In such vertical conveyance, the stand-pipe extends through a wall of the tank and is connected inside the tank to the upper end of a conveyor nozzle which is itself mounted over the aeration plate through which the campressed air is introduced into the tank. The fine material inside the tank is thus loosened and, when suspended in the air, behaves like a fluid and ascends the stand-pipe under the action of the air pressure. Disadvantages of these prior art devices arise, however, because in the great majority of practical cases pure vertical conveyance is insufficient. While in the container itself the stand-pipe can be mounted vertically over rhe aeration plate, after it leaves the container the vertical direction must eventually be changed into a horizontal one ns in almost all cases the receiving container is not located vertically above the delivering container. In cement transport vehicles, for example, this change of direction is obtained by means of flexible pressure conveyor hoses. Unless special devices are provided on the container, the allowable radius of curvature required for this change of direction is subject to a relatively high minimum value, thereby requiring a large amount of space and careful attention to hose layout. The loss of energy due ;to small curvatures is considerable, with the result that whatever efficiency is gained by using a vertical conveyor system can easily be dissipated by frictional losses caused by sharp changes in direction of the conveyor standpipe or hose. This factor is of particular importance where the delivering container is mounted on a vehicle. A further disadvantage of the vertical arrangement of the conveyor standpipe is the difficulty involved in connect- ing extension pipes or hoses. When the standpipe is mounted vertically above the aeration plate it will extend outwards 'through the top wall of the tank so that a driver or operating crew must climb up on the tank, carrying heavy hoses in order to attach it to the outside end of the stand-pipe.

The present invention avoids a number of the disadvantages of such prior art devices by providing a pneumatic conveying apparatus for the vertical conveyance of dustv or fine grained materials stored or transported in air tight containers, the apparatus itself consisting of a conveyor stand-pipe extending through the wall of the container and being attached on the inside to the converging end of an oblique frusto-conical conveying nozzle, the axis of the conical section being inclined relative to its basal area, which basal area is positioned in a plane parallel to and slightly above the inside surface of the aeration plate through which the compressed air is admitted into the tank. A similarly slanted displace ment cone may be mounted inside the nozzle so that the bases of the tvzo conical members are substantially coplanar, thereby defining an annular nozzle entrance. As compared with previously known ver tical conveyor nozzles, this slanted conical nozzle has ;the advantage of permitting the material to be brought out of the container at a comparatively low level position without sacrificing the advantages gained by the higher efficiency of vertical conveyance methods. This, of course, makes it possible to have the conveyor line emerge from the container at a repoint low enough that the operator standing on the ground can connect the extension pipes or hoses to it without the necessity of climb'ing up on the top of the container. Another advantage of the present invention is that it makes it possible for the conveyor stand~pipe to emerge from the container, not only at a reIatively low level, but also in a substantially horizontal direction so that no sharp ends are needed in the conveyor extension pipes or hoses, thereby reducing the substantial friction losses previously associated with these components. A further advantage arising from the use of the present invention is that the distance between the bottom edge of the conveyor nozzle and the aeration plate can be kept very small so that practically all the material in the container can be discharged by means of the pneumatic conveyor apparatus. A still further advantage of the invention is obtained Iby adjusting the distance between the nozzle and the aeration plate, thus varying the operating characteristics of the conveyor nozzle so as to obtain optimum efficiency of the pneumatic conveyor system for materials of

different density and/or particle sizes. In order that the invention may be clearly understood and readily carried into effect reference is directed to the accompanying drawing, wherein: Figure 1 shows an inclined conveyor nozzle with suitable displacement cones installed in a conical container. Figure 2 shows a conveyor apparatus comprising an inclined conveyor nozzle with a displacement cone, used as a discharging apparatus from a tilting container. Figure 3 shows the structural details of the inclined conical conveyor apparatus, and figure 4 shows a section through plane IVW of Figure 3. In each case, the container, when in discharging position, is closed at the 'bottom by an aeration plate 2 through which compressed air is blown from pressure chamber 3 into the eontainer in order to loosen the material. The conveyor nozzle 4, the conveyor stand-pipe S or 51 and the displacement cone 6 are all mounted on or above the aeration plate 2 as discussed below. Conveyor nozzle 4 is in the form of a frustum of an oblique cone, i.e. its axis is not perpendicular to the base of the cone defining the nozzle aperture. This base is itself parallel to the aeration plate and is situated a given distance above it as best shown in Figure 3. Conveyor stand-pipe 5 or 51 is attached to the upper, converging end of the conical nozzle 4. For this purpose the apex of the cone is cut off at a slant so that, when joined, the longitudinal axis of the conveyor pipe makes an oblique angle with the axis of Ithe conical nozzle. In order to avoid sharp bends projecting into the joint between the nozzle and the stand-pipe which might cause undesirable friction losses, the side of the joint on the short side of the cone is rounded as shown at 7. The conveyor stand-pipe may, as shown in the solid line at 5, extend outwardly through ;the wall of the container with a relatively large radius of ,curvature, or, in the alternative, it may run in a substantially straight line as shown at 51. In each case the standpipe is fitted at its outside end with a valve S or 8' land a fitting 9 or 9t for attaching thereto extension pipes or hoses. Improved operation of the present invention can be obtained with the use of a displacement cone whose apex extends up inside the conveying nozzle so that the bases of the displacement cone and the nozzle define an annular nozzle inlet area 23 as best shown in Figure 4. The use of this displacement cone makes possible a considerable increase in the effective suction area provided by the conveyor nozzle, For the most efficient utilization of energy during discharge of the material,

it is la matter of primary importance not to have the ratio of the area of the conveyor nozzle opening to the cross-sectional area of conveyor stand-pipe exceed a certain fixed amount This means that the area of the nozzle opening should he kept comparatively small, which in turn greatly reduces the 'area of the bottom of the container over which effective suction action is exerted by the nozzle. The displacement cone inside the conveyor nozzle allows the designer to increase the outside circumference of the nozzle without increasing the area of the actual nozzle opening and hence the ratio of that area to the cross-sectional area of the stand-pipe. The increased suction range thereby obtained, i.e. the increase in the area on the bottom of the contrainer subjected to suction effect, allows a reduction in the height of the container, thus giving it a lower centre of gravity. This latter advantage is of considerable importance an the case of mobile containers. Such a displacement cone, indicated at 6, may most conveniently have a similar obliquity to the nozzle and is paced directly on the aeration plate 2. It is preferably eccentrically situated inside nozzle 4 so that the gap between the nozzle and displacement cone is narrower on the short side of the cone than lon the long side (see Figures 3 and 4). The eccentric mounting of this displacement cone secures uniform discharge of material on all sides. It will be obvious that on the shorter side of the conveyor nozzle withe material is discharged more rapidly than on the longer side. With a concentric arrangement of the displacement cone inside the nozzle, the discharge process is liable to continue only until the bottom end of the conveyor nozzle stands free on its shorter side, with the result that a complete discharge of the material from the container would not be achieved. Th the caseof a displacement cone of similar obliquity to the conveying nozzle, it will of course be desirable to have the axis of the displacement cone and the nozzle parallel to each o.ther, the term " axis," as 'applied to a cone, denoting the line joining the centre of the base and the apex, and the work "parallel" including the condition of co-incidence of the two axes, unless otherwise specifically excluded. When the nozzle and displacement cone have similar obliquity, but the latter is eccentrically mounted inside the former, the axis ,o the displacement cone will ibe parallel to but laterally-displaced from the axis of the nozzle in a direction toward the shorter side of the nozzle so that the narrowest part of the annular inlet area will be located at the shortest side of the nozzle. Figure 2 represents a tilting container fitted with a conveyor apparatus in accordance with the invention. Aeration plate 10 is mounted in the lower corner of the tilted container.

Space 11, formed between the 'aeration plate and the wails of the container serves as a pressure tank for the aeration air. The oblique frusto-coniical conveyor nozzle 12 is mounted a suitable distance above the laeration plate 10. The apex of the conical nozzle 12 is cut off at a slant and conveyor pipe 13 formed with a relatively large radius of curvature, b attached to the upper converging end of the nozzle, the ,other end of the conveyor pipe projecting from the rear wall of the container where it is provided with a valve 14 and fitting 15. As in Figure 1, conveyor pipe 13t can lalso ge straight as shown in ithe dashed lines at 131. Displacement cone 16 is again mounted directly on the aeration plate 12 and has the shape of anl oblique cone. Analogous to the oanstruotion shown in Figure 4 which illustrates the special case of a circular base design, the makes of the conical nozzle and the displacement cone are laterally displaced with respect to each other. In the emibodiments shown' in Figure 2 the bases of the displacement cone 16 and conveyor nozzle 12 have the same shape as the aeration plate which, in this case, is preferably oval. Figure 3 gives the details of the invention as shown it' Figure 1, together with an improvement thereon. Here container 1 is closed off at the bottom by aeration plate 2 and is provided with compressed air tank 3. Displacement cone 6 is placed directly on aeration plate 2. It has the form of an oblique cone, i.e. its axis is not perpendicular to the laeration plate. The base of the displacement cone is In this case 'circular. 'Conveyor nozzle 4 is placed over the cone in such a way that gap 17 is left between it and the aeration plate 2. conveyor nozzle 4 like displacement cone 16, is in the form of an oblique cone with a eircular base. The apex lof the cone is cut off at a slant (indicated by th,e dash lines) allowing the upper converging ends d the ozone to be attached to the inside end of slightly curved conveyor pipe 5 which extends outside container 1. As disclosed above, conveyor nozzle 4 and displacement cone 6 are eccentrically aligned with respect to each other as best shown in Figure 4, so that the igap tbe- tween then is narrower at the shorter side of the cone than it is at the longer side. The actual distance between these two parts is adjusted by means of a suitable holding device PX. The minimum distance is determined by the size of spacers 19' which are attached to the displacement cone and which make contact with the conveyor nozzle at the desired minimum limit of distance between them. Since conveyor nozzle 4 is moved vertically in order to adjust this distance, conveyor pipe 5 must be made movable, but airtight, by mounting it jn stuffing box 20 in the container wall. Outside container 1 conveyor pipe 5 has fitted therecn valve 8 and a fitting 9. figure 4 illustrates the apparatus shown in

Figure 3 as sectioned along IV-IV and emphasizes the eccentric position of displacement cone 6 within conveyor nozzle 4. Displacement cone 6 rests on aeration plate 2, which is closed off from the outside by wall 22 of the container Conveyor nozzle 4, ithe bottom parr of which is represented in this Figure is situated above displacement cone 6. conveyor stand-pipe 5, indicated by dashed lines, is attached to the top of conveyor nozzle 4 on the side at which the gap between it and displacement cone 6 is narrowest. in all cases the shape of the basal area of the conveyor nozzle and that of the displacemeat cone should conform to that of the aeration plate. Where the plate is circular, as in the case of conical containers, the basal areas of the conveyor nozzle and displacement cone should also be circular. If the aeration plate is oval or ellipsoidal, as in the case of tiltable containers or the like which are tipped on one edge during evacuation, the basal area of the conveyor nozzle and displacement cone should rst > also be oval or ellipsoidal as the case may be. The advantage of this arrangement is that material lying on the aeration plate will always be taken up and discharged unifirmly by the suction of the conveyor nozzle. The point of attachment of the conveyor stand-pipe to the conveyor nozzle is at the upper, converging end of the conical conveyor nozzle, and the plane in which the joint b made can be either perpendicular to the axis of the cone or at an angle to rt. In the latter case, or where the actual join is in a plane perpendicular to the axis of the nozzle but the conveyor pipe approaches at an angle to the axis, care should be taken to ensure that no sharp bends occur at the join which might detract from the power saving effect gained from the use of a vertical conveyor system. Attachment of the conveyor stand-pipe at an angle to the axis of the nozzle, as shown in the anbodiments illustrated by the drawings, has the advantage that the curvature of the conveyor pipe within the container becomes smaller and the pipe emerges from the container at a lower point. 'Whaticlaimis:- 1. Pneumatic conveyor apparatus for the conveyance of fine-grained material, said apparatus comprising a container holding the material, an aerating plate mounted at the bottom of the container, a conveyor stand-pipe extending into the container and connected to the converging end of an oblique frusto-conical conveying nozzle, the basal area of said nozzle being positioned parallel to and slightly above said aerating plate. 2. The apparatus as claimed in claim 1, comprising a displacemett cone whose apex extends upwardly inside the conveying nozzle, thereby

forming an annular nozzle inlet area. 3 The apparatus as claimed in claim 1, comprising a displacement cone of similar obliquity to the conveying nozzle, the apex of the displacement cone extending upwardly inside the conveying nozzle, thereby forming an annular nozzle inlet area. 4. The apparatus as claimed in claim 2, wherein the bases of the nozzle and displacement cone are substantially co-planar. 5. The apparatus as claimed in claim 3, wherein the bases of the nozzle and displacement cone are substantially co-planar. 6. The apparatus as claimed in claim 3, wherein the axis of the displacement cone is parallel to the axis of the conveying nozzle. 7. The apparatus as claimed in claim 5, wherein the axis of the displacement cone is parallel to the axis of the conveying nozzle. 8. The apparatus as claimed in claim 3, wherein the axis of the displacement cone is parallel to but laterally displaced from the axis of the conveying nozzle in a direction toward the shorter side of the nozzle. 9. The apparatus as claimed in claim 5, wherein the axis of the displacement cone is parallel to but laterally displaced from the axis of the conveying nozzle in a direction toward the shorter side of the nozzle. 10. The apparatus as claimed in claim 1 in which the apex of a displacement cone of similar obliquity to the conveying nozzle extends upwardly into the conveying nozzle, thereby forming a substantially annular nozzle inlet area, and means whereby the position of the conveying nozzle is vertically adjustable so as to allow variation of the nozzle inlet area. 11. The apparatus as claimed in claim 10, wherein the axis of the displacement cone is parallel to the axis of the conveying nozzle. 12. The apparatus as claimed in claim 10 wherein the axis of the displacement cone is parallel to but laterally displaced from the axis of the conveying nozzle in a direction toward the shorter side of the nozzle. 13. The apparatus as claimed in any of claims 2, 3 or 4 in which the basal area and cross-section of both the conveying nozzle and displacement cone are circular. 14. The apparatus as claimed in any of claims 5, 6 or 7 in which the basal area and cross-section of both the conveying nozzle and displacement cone are circular. 15. The apparatus as claimed in any of claims 8, 9 or 10 in which the basal area and cross-section of both the conveying nozzle and displacement cone are circular. 16. The apparatus as claimed in either of claims 11 or 12 in which the basal area and cross-section of both the conveying nozzle and

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