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1. * GB786004 (A)
Description: GB786004 (A)
No title available
Description of GB786004 (A)
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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withdrawn in the liquid form therewith.

2. 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

3. 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
Description of GB786005 (A)
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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
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.

4. 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

5. 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

6. 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

7. 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

8. 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

9. 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

10. 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.

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* GB786006 (A)
Description: GB786006 (A) ? 1957-11-06
Primary aliphatic amines and/or their hydrohalides and process of producing
the 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

12. 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-pro- duct
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

13. 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

14. 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

15. 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

16. 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., respec- tively, 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

17. 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

18. 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

19. 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
Description of GB786007 (A)
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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
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

20. 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

21. 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.
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* 5.8.23.4; 93p
* GB786008 (A)
Description: GB786008 (A) ? 1957-11-06
Conveyor apparatus for the evacuation of dusty or grain material from
pressure tanks by means of compressed air

22. 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 par-
ticularly, 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 down- wards 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

23. 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 im-
portance 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.

24. 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

25. 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,

26. 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 in- crease 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 obli- quity 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-dis- placed 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.

27. 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 pro- jecting 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

28. 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

29. 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