4936 4940.output

* GB785343 (A)
Description: GB785343 (A) ? 1957-10-23
Improvements in adjustable sieves
Description of GB785343 (A)
PATENT SPECIFICATION
785,343 em Date of Application and filing Complete SpecificationJune
21, 1955.
No 17977/55.
Application made in South Africa on June 25, 1954.
Complete Specification Published: Oct 23, 1957.
Index at acceptance:-Classes 8 ( 2), D 3 (C: D 2: D 4: DX: E 1 X: E 2
F); and 117, B 2 (A: B: F: G: H:
M).
International Classification:-B Old B 02 f.
COMPLETE SPECIFICATION
Improvements in Adjustable Sieves 1, ERNEST MARE, of 902, S A Fire
House, Corner of Marshall and Harrison Streets, Johannesburg,
Transvaal Province, Union of South Africa, a South African Citizen, do
hereby declare the invention, for which I pray that a patent may be
granted to me, and the method by which it is to be performed, to be
particularly described in and by the following statement: -
This invention relates to screens for size separation of solid
particles or the removal of discrete particles of small size carried
in a gaseous current It is particularly applicable to the screening of
particles from air and the 1 S invention will be described when used
for such a purpose.
In woven screens such as cloth screens the open area is limited to
that unoccupied by the crossed filaments woven to form a mesh.
Such screens are easily clogged and not easily cleaned particularly
when screening particles of very small size To avoid this loss in area
and assist in cleaning a screen has been made, known as the Heller
screen, consisting of steel wires laid parallel and without cross
wires This type of screen is, however, not suitable for screening very
small particles and it is the object of the invention to provide a

screen suitable for removing very small particles, 50 microns or less
from an air stream.
According to this invention there is provided a screen consisting of
smooth flexible tensioned filaments substantially uniform in diameter,
assembled parallel to one another in one fiat plane with the widths of
the spaces between the filaments in said plane being less than 50
microns, said filaments extending between supports allowing individual
vibration of said filaments.
According to a further feature of this invention the efective width of
the spaces netween the filaments is varied either by vibrating them
and at varying amplitudes, or by varying their cross sectional area by
stretching them or by stretching the members of the F Plie frame on
which they are wound.
According to still further features of the invention the filaments may
be made of ferro-magnetic material, and the vibration 50 effected by
an oscillating magnetic field; it is also provided that the screen may
be made double by vwinding the filaments over the outside of the
frame, the distance between the two screens depending on the thickness
of 35 the two sides of the frame over which the filaments are wound,
and that the filaments may be thickened by heating or they may be
given a covering by wetting them.
For the purpose of description the accom 60 panying drawings
illustrate diagrammatically the invention in which: Fig 1 is a front
elevation of a portion of the screen.
Fig 2 is an end elevation of the screen 65 Fig 3 illustrates one means
for vibrating the screen.
Fig 4 illustrates a means for cleaning the screen.
Figs 5 and 6, show details described here 70 inafter.
In the drawings 10 represents the frame of the screen, which may
consist of the two end members 11, 11 These end members 11, 11 are
joined by rods 12 threaded through lugs 7 13, 13 fixed at the ends of
members 11, 11.
The members 11, 11 may be made of metal.
wood, hard rubber, plastic or like material.
The rods 12 are screw threaded and provided with nuts 14, 14, which
are made to 80 butt against the lugs 13, 13, to keep the members 11,
11, apart and so put a tension on the filaments making up the screen.
In the form of the screen shown the fiia ments making up the screen
are wound 85 around the frame members 11 so that the strands are close
together and form practically a continuous surface.
Considering in the first case that the filament is a ferro magnetic
wire, an electro 9 g magnet 16 (Fig 3) may be placed in the frame
between the filaments, and, when activated by a pulsating current,
will vibrate them The extent of the vibrations will be a measure of

the spaces between thie filaments and consequently the coarseness or
the sieve At the same time tie amplitucie of the vibrations will
dnepernd on the eiion of the filaments 15 which may be regulated by
the nuts 14, or by the intensity of tle cur rent passing through the
electro magnet 165.
i O It will be obvious that the wire or other filaiment used in the
construc ion of the screen should be selected from those gauges which
are obviously practical for such use, that is gauges which provide
sufficient L Ehi Ck1 S ness to withstand the tensioning contemplated
by the invention yet sufienly fileible to vibrate readily -It will be
further understood that since tie screen is required to remove
particles of 50 microns or less under dry screening conditions the
spaces between the filaments when they are in one fiat plane swill be
appreciably less than 50 microns as during -vibration of the filaments
the spaces between will increase to an extent depending on their
degree of tensioning Under wet screening conditions if the spaces are
less than 50 microns apart when the filaments are in one flat plane in
spite of the spaces increasing during vibration they will still screen
particles of under 50 microns diameter due to the films of water which
form on the filaments increasing the effective diameter of the latter
and thus decreasing the effective widths of the spaces between them
The filaments must also be smooth and of uniform diameter, as would be
the case with normal metal wires, to avoid variation in the
effectiveness of different parts of the screen which would result from
non-uniforra or irregularly shaped wires.
In screening dust laden air, water sprays from a duct 17 may be
directed onto the screen as shown in Figure 4 Due to the small width
of the spaces between the filaments and the surface tension of the
water the latter appears largely to fill the spaces between the
filaments and entrap the dust particles The water then flows in a
turbulent manner down the downstream side of the screen with the
entrapped dust particles and into a reservoir leaving the air
substantially free of both dust and water particles.
The filament made, as already described, or if formed of glass or
similar fibre may be thickened by heating or by a coatinu of liquid If
the filament is a conductor the heating may be effected by the passage
of an electric current as shown in Fig 5, where 18 represents the ends
of the wound filament which may be connected to an electric current
supply If a coating of liquid is used, a supply may be furnished from
perforated pipes 19,20 19 is placed on the outside and 20 on the
inside of the double screen.
Mechanically produced bhiws may be imparted to lne frime to set up
Vibra ions or again Stle strech Ied strands mnay be made throu GI 1
e-, l; lc W o vibrate ii zs-xpathy with su'tab-e sounc 1 i Waves Und

certain 70 ccnldito>-_ tme o i-l-4 is 1 11 af the mole whrken made of
suit vie nxterial are capable ofr sbi c sretooed linarv S and so
ircrease the uh's One U ' -'-?in the s-r' of 'he filament olijd c l
them 75 It bil be ti' ierstoc'l herefore that the -,ibration of th I
wires m'lay be effected by the passfie c r'r be"-se thrvl adjor by
mechanical, electcal or "onic means The screen 1 v bco 7 mne e I
Tectively coarser the 80 greater the aniritvude of vibration Other
factors being equal the amplitude of vibration will decrease with
increase in tension of the strands since all the strands will not
vibrate in unison or at exactly the same am 85 31 itude.
In practice the two factors affecting the eflective coarseness of the
screen namely the cross sectional area of the strands and the
amplitude of vibration will be, to a greater or 90 lesser degree,
interdependent depending on the type of material used for the
filaments since both factors depend on the tension of the filaments.
The invention has been described and 95 shown as a sieve with a double
screen but a single layer of filaments may be used This may be done by
securing the strands at one end to the frame and clamping the opposite
ends between a pair of bars which are rota 100 ted about fixed centres
so that the strands are wound up on then Alternatively the bars may be
drawn towards or allowed to move away from a fixed end of the frame of
the screen by means of nuts 14 on rods 12 10 or like -means.
In both cases the strands may be brought around a strip of rubber or
like flexible material attached to the side of one of the members 11
which will act to equalise the 110 tension in the strands.
To make up a sieve with a single screen the filament may be wound
round the frame 11, 11, and then strips 21, Fig 6 securely fastened to
the strands 15 by soldering or 115 otherwise afterwards they are cut
between the strips 21 to provide two lots of strands which may be
mounted to form a screen in any suitable manner.
Iti will be seen, wiih a screen according to 120 this invention, that
it is possible to obtain the minute variations in she effec Live width
of the spaces beta en the filaments which are necessary when dealing
with particles of very small size It ill also be seen that the 125
screen iv self cleaning o, may be easily cleaned by brushin or by a
hio-w; ol a aas or liquid theretlhroualh or by heating the wires, if
tale material on the screen is combustible and the filarnents
incombustible 130 785,343 wherein an electromagnet is used to vibrate
the filaments.
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* 5.8.23.4; 93p
* GB785344 (A)
Description: GB785344 (A) ? 1957-10-23
Improvements in or relating to production of vanadium metal
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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 7 X'
Inventors:-JOHN STEWART BROADLEYand CHRISTOPHER TYZACK.
Date of filing Complete Specification: June 20, 1956.
Application Dale: June 23, 1955 No 18159155.
(Complete Specification Published: Oct 23, 1957.
Index at Acceptance:-Class 82 ( 1), I( 4 A 2: 4 A 3 C 13).
International Classification:-B 22 b.
COMPLETE SPECIFICATION.
Improvements in or relating to Production of Vanadium Metal.
56)344 We, UNITED KINGDOM ATOMIC ENERGY AUTHORITY, London, a British
Authority, do hereby declare the invention, for which we pray that a
patent may be granted to us, and the method by which it is to be
performed, to be particularly described in and by the following
statement:-
This invention relates to the production of vanadium metal and it is
concerned with the hydrogen reduction of the trichloride of vanadium
to produce vanadium metal.
In the course of the hydrogen reduction of vanadium trichloride a
degree of dispro.

portionation to the tetra and di-chlorides 1,5 inevitably occurs and
this disproportionation represents a loss in reduction efficiency due
to the escape of the very volatile tetrachloride of vanadium.
According to the present invention vanadium trichloride is reduced by
hydrogen in two stages, the first stage comprising a reduction at a
temperature in the range 400-500 O C and preferably at about 450 C and
the second stage a reduction at 25) a temperature in excess of 950 C.
The following is an example of one way of carrying the invention into
effect.
EXAMPLE.
A silica tube furnace having an inlet at one end for admission of
hydrogen gas, and an outlet at the other end which was connected to a
silicone oil trap and an extractor Hydrogen was supplied to the inlet
by way of a flowmeter, a magnesium perchlorate drying tower, a column
packed with uranium turnings held at 750 C and finally an evacuating
T-joint Vanadium trichloride was filled into a molybdenum boat, the
operation being carried out in an lPrice 3 s 6 d l atmosphere of pure
argon and the transfer of the boat to the furnace being under counter
current of hydrogen.
The temperature of the furnace was raised to 4500 C and hydrogen was
allowed to flow into the furnace at a rate of 50 litres per hour for a
period of 24 hours The temperature of the furnace was then raised to
10000 C and hydrogen flow was continued for a further 24 hours A yield
of 80 per cent of the theoretical was obtained.
Experimentation has shown that the speed of reduction is increased
with increased flow rate and improved gas-solid contact The economies
of the reduction could be improved by using a fluidized bed of
vanadium tn-chloride through which is passed hydrogen in a closed
cycle at a fast rate with a small make-up feed.
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* GB785345 (A)
Description: GB785345 (A) ? 1957-10-23

New monoazo dyestuffs of the benzene-azo-naphthalene series and metal
complexes thereof
PATENT SPECIFICATION
785,345 Date of Application and filing Complete Specification: June
28, 1955.
No 18670155.
Application made in Switzerland on June 29, 1954.
Complete Specification Published: Oct 23, 1957.
Index at acceptance:-Class 2 ( 4), P 1 (A 2 A 2: D 2: F 1: Fib F 6), P
8 (A 1 A: A-IC: B 1: Cl C 2: C 3: E), P 9 A 4 B. International
Classification:-CO 9 b.
New Monoazo Dyestuffs of the Benzene-Azo=Naphthanene Series and Metal
Complexes thereof We, SAN Doz LTD, of Basle, Switzerland, a Body
Corporate organised according to the laws of Switzerland, 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
The present invention relates to a process for the preparation of
monoazo dyestuffs and their metal complex compounds The process
consists in coupling 1 mol of the diazo compound derived from a
2-amino-1-hydroxy or -methoxy-benzene with 1 mol of a
1-hydroxyacylamino 7 hydroxynaphthalene of the is formula A'/-d x
-a>/yknyee -06 ' O wherein x denotes a simple linkage or -OCH 2- A
preferred coupling component is 1-hydroxyacetylamino
7-hydroxynaphthalene The monoazo compounds obtained can be treated
with metal-yielding agents in substance or on the fibre.
The new dyestuffs in the metal-free state have the general formula Uf
O wherein x has the above defined significance and R denotes a residue
of the benzene series which contains a hydroxy or methoxy-group in the

ortho position to the azo linkage.
For the preparation of the diazo compounds the following amines for
example can be used, lPrice 3 s 6 d l 2-amino 1 hydroxybenzene, 2
amino-lhydroxy-halogenbenzenes, 2-amino-1-hydroxynitrobenzenes,
2-amino-l-hydroxy-halogennitrobenzenes,
2-amino-1-hydroxy-acylaminohalogenbenzenes, 2-amino
1-hydrox-y-acylamino-nitrobenzenes, also the large series of
2amino-l-hydroxybenzenesulphonamides, their derivatives further
substituted on the nitrogen atom of the sulphonamide group by alkyl,
halogenalkyl, hydroxyalkyl, alkoxyalkyl, aralkyl, carbocyclic and
heterocyclic residues, 2-aminoponding 2-amino-1-methoxy compounds.
Specially valuable are 2-amino-1-hydroxybenzene-4-sulphonamide,
2-amino-1-hydroxybenzene-4-sulphonmethylamide,
2-amino-1hydroxybenzene-4-sulphonic acid-( 21-hydroxy) ethylamide,
2-amino 1-hydroxybenzene-4sulphonic acid-( 31-methoxy)-propylamide,
2amino-l-hydroxybenzene 4 sulphonbenzylamide,
2-amino-1-hydroxybenzene-4-sulphoncyclohexylamide and 2
amino-l-hydroxybenzene-4-sulphonphenylamide which can be further
substituted on the phenylamide residue e.g by a carboxyl, acylamino,
sulphonamide, sulphonmethylamide and sulphondimethylamide group united
to the nucleus, and also 2-amino-1-hydroxy-4-methylsulphonylbenzene.
The most important 1-hydroxyacylamino-7hydroxynaphthalenes as herein
defined are 1hydroxyacetylamino-7-hydroxynaphthalene and 1-carbo-(
21-hydroxy)-ethoxyamino-7-hydroxynaphthalene They are obtained from
the corresponding chloracylamino compounds by heating to high
temperatures such as 160 C.
in formamide.
The coupling takes place advantageously in an alkaline medium; the
working up and isolation of the products obtained takes place in the
usual way.
Wool can be treated with the metal-free monoazo dyestuffs and by an
after-metallising or single-bath-metallising process gives shades
which are fast to washing, milling and light.
In this way blue-grey and grey to olive shades are obtained with
chromium-yielding agents and blue to grey shades are obtained with
cobalt-yielding agents.
For the conversion of the metal-free dyestuffs into the metal-complex
compounds, chromium-yielding and cobalt-yielding agents come
particularly into consideration Agents of this kind are for example,
salts of chromium, e g chromium fluoride, chromium sulphate, chromium
formate, chromium acetate, potassium or ammonium chromium sulphate,
and sodium or potassium chromate or bichromate and the salts of
cobalt, e g cobalt acetate, cobalt formate and cobalt sulphate The
metallisation takes place advantageously in aqueous suspension or

solution, or in an organic medium, as for example formamide or in the
melt of an alkali metal salt of a lower molecular aliphatic
monocarboxylic acid In the latter case, insoluble heavy metal
compounds can also be used as for example cobalt hydroxide and cobalt
carbonate Metallisation in aqueous caustic alkaline medium is
particularly advantageous, whereby the metal salts are added in the
presence of such compounds as have the property of keeping chromium
and cobalt in the dissolved form in a caustic alkaline medium, as e g
tartaric acid, citric acid, and lactic acid If the monoazo dyestuffs
contain an ortho-hydroxy-orthol-methoxy-azo grouping, then the
metalisation takes place with splitting off of the methoxy group This
is carried out by heating the dyestuff to a higher temperature in an
organic medium, as for example in a glycol (e g ethylene glycol,
butylene glycol, ethylenepolyglycol) The metallisation of the monoazo
compounds takes place in all cases in such a way that for 1 mol of the
monoazo compound less than one atom of the metal is taken up In this
way there are formed for example the so-called 1:2 complexes which for
2 mols of the monoazo compound contain approximately one atom of
metal.
The metal-containing azo dyestuffs produced are separated from the
aqueous medium by addition of salt, when necessary, after pouring the
organic metallising solution into water and are thereupon filtered
off, washed if desired and then dried They possess an outstanding
power of exhaustion for wool from neutral baths; they dye wool even
from a neutral bath, and silk and Tursore from weakly acid baths in
blue-grey and grey to olive shades of very good fastness to washing,
milling and light.
They are also suitable for dyeing leather and are suitable very
especially for dyeing artificial nitrogenous fibres such as polyamide
fibres W O (e g Nylon and Perlon) Their ready solubility in polar
solvents such as acetone, dimethylformamide and tetrahydrofurane
furthermore enables them to be used for the dyeing of artificial
fibres which are spun from organic solvents (e g acetate rayon or
polyester fibres).
In many cases mixed metal complex compounds obtained from the
metallisation of mixtures of 2 or more monoazo dyestuffs as defined in
this invention surpass the single metal complex compounds in their
dyeing properties 70 Mixed metal complex compounds of this kind form a
further object of the present invention.
The following examples illustrate the invention without limiting it
Therein the parts denote parts by weight, the percentages, per 75
centages by weight and the temperatures are given in degrees
Centigrade.
EXAMPLE 1.

20.2 parts of 2-amino-1-hydroxybenzene-4sulphonmethylamide are
diazotised in a mix 80 ture of 20 parts 30 % hydrochloric acid and 100
parts of water at 0-5 with a solution of 6 9 parts of sodium nitrite
in 30 parts of water.
The diazo suspension is coupled at 0-5 with a solution of 22 parts of
1-hydroxyacetyl 85 amino-7-hydroxynaphthalene in 6 parts of sodium
hydroxide, 20 parts anhydrous sodium carbonate, 350 parts of water and
10 parts of a technical mixture of pyridine bases The product is
vigorously stirred for some hours at 90 0-5 At the end of this period
the coupling is completed and the monoazo dyestuff which has separated
out almost completely is isolated in the known manner In the dry and
ground state it is a dark violet powder which dissolves 95 in water
with a violet colour and in a concentrated sulphuric acid with a
Bordeaux red colour Its dyeings on wool by the after-chroming process
or the single-bath chroming process are grey and show a very good
fastness to 100 washing, milling and light.
The new coupling component used for the preparation of the monoazo
dyestuff in this example can be obtained by heating
1-chloracetylamino-7-hydroxynaphthalene in form 105 amide for several
hours at 160-180 .
EXAMPLE 2.
21.6 parts of 2-amino-1-hydroxybenzene-4sulphonmethylamide are coupled
with 25 parts of 1-carbo-( 21 hydroxy) ethoxya Tnino-7 110
hydroxynaphthalene according to the data of the foregoing example A
dyestuff very similar to that described in Example 1 is obtained.
The coupling component used in this example is obtained by heating
1-carbo-( 21-chlor) 115 ethoxyamino-7-hydroxynaphthalene for several
hours in formamide at 160 .
EXAMPLE 3.
43 parts of the monoazo dyestuff obtained according to Example 1 are
dissolved in 1,500 120 parts of water The solution is treated with 16
parts of sodium bichromate and is boiled under a reflux condenser
until complex formation is ended which requires several hours The
chromium-containing azo dyestuff after 125 separating out, filtering
off and drying is a dark powder which dissolves in water with a blue
colour and in concentrated sulphuric acid with a red colour It dyes
wool, silk and synthetic polyamide fibres in blue-grey shades 130
785,345 according to Example 1 are dissolved in 800 parts of warm
water, the solution is treated with a mixture of 28 2 parts of
cobaltous sulphate, 7 6 parts tartaric acid, 35 parts of % sodium
hydroxide solution and 350 parts of water The complex formation ensues
immediately The cobalt-containing azo dyestuff is separated off,
filtered off and dried It dyes wool, silk and synthetic polyamide
fibres in reddish-grey shades of very good fastness properties.

EXAMPLE 7.
21.5 parts of the monoazo dyestuff obtained according to Example 1 and
23 parts of that obtained according to Example 2 are dissolved in
1,000 parts of water at 900 with the help of 30 parts of 30 % sodium
hydroxide solution.
The solution is treated with 80 parts of hot % aqueous cobaltous
sulphate solution After complex formation is completed, the cobalt
containing azo dyestuff is separated off, filtered off and dried It
dyes wool, silk and synthetic polyamide fibres in blue-grey shades of
excellent fastness to washing, milling and light.
The following Table 1, shows further metalcontaining azo dyestuffs
which can be obtained according to the methods shown in the previous
examples For their characterisation Column (A) shows the
2-amino-1-hydroxy or -methoxybenzenes used for the preparation of the
diazo compounds, Column (B) shows the 1-hydroxyacylamino 7
hydroxynaphthalenes used as coupling components and Columns (C) and
(D) the colour of the dyes on wool with the chromium-containing or
cobalt-containing azo dyestuffs respectively.
of excellent fastness to washing, milling and light.
EXAMPLE 4.
21.5 parts of the monoazo dyestuff obtained according to Example 1 and
23 7 parts of that obtained according to Example 2 are dissolved in
1,000 parts of water at 900 with the help of 6 parts of sodium
hydroxide To the dyestuff solution there is then added a solution of
24 parts of sodium bichromate and 4 parts of sodium hydroxide and 100
parts of water and finally 80 parts of a 20 % aqueous dextrose
solution The temperature of the metallising solution is maintained at
90-95 until the complex formation is completed, and the
chromium-containing azo dyestuff isolated and dried It dyes wool, silk
and synthetic polyamide fibres in blue-grey shades of excellent
fastness to washing, milling and light.
EXAMPLE 5.
44.4 parts of the monoazo dyestuff obtained by coupling 21 6 part sof
2-amino-1methoxybenzene-4-sulphonmethylamide with 22 parts of
1-hydroxyacetylamino-7-hydroxynaphthalene according to Example 1, are
dissolved in 400 parts of ethylene glycol 50 parts of potassium
chromium sulphate are added to the solution which is then warmed to
1400 until completion of the complex formation The reaction mass is
poured into 1200 parts of water, the chromium-containing azo dyestuff
salted out, filtered off and dried It is identical with the product
obtained according to Example 3.
EXAMPLE 6.
43 parts of the monoazo dyestuff obtained Example No.
(A) 2-amino-1-hydroxy-4methylsulphonylbenzene

2-amino-1-hydroxybenzene-5-sulphonamide
2-amino-1-hydroxybenzene-4-sulphon-( 21hydroxy)-ethylamide
2-amino-l-hydroxybenzene-4-sulphon-( 31methoxy)-propylamide
2-amino-l-hydroxy-4chlor-5-nitrobenzene
2-amino-1-hydroxybenzene-4-sulphon-( 31sulphonmethylamido)phenylamide
TABLE 1 (B) 1-hydroxyacetyl-amino7-hydroxynaphthalene (C) bluegrey (D)
violetgrey bluegrey reddishgrey 1 785,345 785,345 TABLE 1-coztinued
Examkple I (A) I(B) (C) j (D) No 1 I 1 rdih
2-amino-1-hydroxybenzene-4-sulphon-( 31sulphamido)-phenylamide
2-amino-1-hydroxybenzene-4-sulphon-( 31acetylamino)-phenylamide
2-amino-1-hydroxy-4chlorbenzene I 2-amino-1-hydroxy-5nitrobenzene 1
2-amino-1-hydroxy-4chlor-6-nitrobenzene | 2-amino-1-hydroxy-4I
nitrobenzene 2-amino-1-hydroxybenzene-4-sulphon-(
21methoxy)-ethylamide 2-amino-1-hydroxy-4nitro-6-acetylaminobenzene
2-amino-1-hydroxybenzene-4-sulphonamide
2-amino-1-hydroxybenzene-4-sulphon-( 21sulphodimethylamido)phenylamide
2-amino-1-hydroxy-5nitrobenzene 2-amino-1-hydroxybenzene-4-sulphon-(
11ethyl-21-hydroxy)ethylamide 2-amino-1-hydroxybenzene-4-sulphon-(
41sulphomethylamido)phenylamide 2-amino-1-hydroxybenzene-4-sulphon-(
21hydroxy)-propylamide 2-amino-1-hydroxybenzene-4-sulphon-dil(
21-hydroxy)-propyllamide I 1-hydroxyacet 5,y
1-amino7-hydroxynaphthalene , , I 1-carbo-( 21-liydroxy)e
Lhoxy-amino-7hydroxynaphthalene ,
1-hydroxyacetyl-amino7-hydroxynaphthalene bluegrey , , , olivegrey
bluegrey olive bluegrey greddish grey bu grey blue grey reddishgrey
|blue grey , reddishgrey l I 1 i 1 1 1 1 i 1 i 1 I 1 I 1 i 1 i 1 1
785,345 TABLE 1-continued (A)
2-amino-1-hydroxybenzene-5-sulphonmorpholide
2-amino-1-hydroxybenzene-4-sulphonethylamide
2-amino-1-hydroxybenzene-4-sulphondiethylamide
2-amino-1-hydroxybenzene-4-sulphonpyrrolidide
2-amino-1-hydroxy-4methyl-6-acetylbenzene
2-amino-1-hydroxybenzene-4-sulphoncyclohexylamide
2-amino-1-hydroxybenzene-4-sulphonbenzylamide
2-amino-1-hydroxybenzene-4-sulphon-( 21hydroxy)-ethylamide
2-amino-1-hydroxybenzene-4-sulphon( 21-methoxy)-ethyl-amide
2-amino-1-hydroxybenzene-4-sulphon( 31-methoxy)-propyl-amide
2-amino-1-hydroxybenzene-4-sulphon( 21-hydroxy)-propyl-amide Table 2
shows metallised mixed complex compounds from two monoazo dyestuffs
which can be prepared according to the data given in Examples 4 and 7
The metallised mixed complex compounds are characterised by the
content of metal-free monoazo dyestuffs which are reacted with one
atom of metal They con(B) 1-hydroxyacetyl-amino7-hydroxynaphthalene
1-( 21-hydroxy)propionylamnino-7hydroxynaphthalene 1-( 3

'-hydroxy)butyrylamino-7hydroxynaplithalenene 1-carbo-(
31-hydroxy)propoxyamnino-7hydroxynaphthalene 1-carbo-( 4
'-hydroxy)butoxyamino-7hydroxynaplithalene (C) bluegrey (D) reddish
grey tain for one atom of metal, about two mols of the mixture of the
two monoazo compounds 10 Column (E) gives the metal used for
metallising the mixture, and Column (F) gives the shade of the dyeings
obtained on wool with the new metal-containing azo dyestuffs.
Example No.
785,345 TABLE 2 r First metal-free | Second metal-free l l Ex morloazo
dyes-cuff monoazo dyestuff ample (E) (F) No Mol As in Example Mol As
in Example 1 1 1 8 Cr blue-grey 41 1 1 1 10 | Cr |, 142 1 1 11 11 1 Cr
| I i 43 1 1 5 1 0 51 11 | Cr |, 144 | 1 2 1 11 Cr 1 | 45 | 1 2 1 1 22
Cr 1 46 1 10 1 11 Cr 1 47 1 5 11 0 5 15 Cr 48 15 11 0 5 16 Cr 49 1 2 1
22 Co reddishI I grey 11 9 1 10 Co I 51 1 1 10 1 20 Co 52 I 1 10 1 22
Col which was then brought to the boil for half an hour After this
operation the dyeing was chromed; it was then rinsed and dried.
EXAMPLE 55.
In a dyebath consisting of 1 part of the chromium-containing azo
dyestuff obtained according to Example 3, 4,000 parts of water and 5
parts of ammonium sulphate, there are entered 100 parts of wool at 40
The bath is heated within half an hour to boiling and maintained at
boiling for 1 hour After cooling down for a short while, the dyed wool
is taken out of the bath, rinsed and dried.
Synthetic polyamide fibres are dyed in the same manner as wool Silk is
dyed at a somewhat lower temperature as for example 95 .
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* GB785346 (A)
Description: GB785346 (A) ? 1957-10-23
Process for the manufacture of isonicotinyl hydrazide

IPATENT SPECIFICATION
Inventor: HERBERT MUGGLETON STANLEY.
Date of filing Cotijplete Specification: June 14, 1956.
1 ppaicationlate: Jine 29, 1955 No 18750155.
Comwplete Specification Published: Oct 23, 1957.
Index at Acceptance:-Class 2,3), C 2 821.
International Classification:-CO 7 d.
COMPLETE SPECIFICATION.
Process for the Manufacture of Isonicotinyl Hydrazide.
We, THE DISTILLERS COMPANY LIMITED, a British Company, 12 Torphichen
Street, Edinburgh 3, Scotland, do hereby declare the invention, for
which we pray that a patent may be granted to us, and the method by
which it is to be performed, to be particularly described in and by
the following statement:-
The present invention relates to a process for the manufacture of
isonicotinyl hydrazide, which is a valuable pharmaceutical product for
combating tuberculosis.
According to the present invention, the process for the manufacture of
isonicotinyl hydrazide comprises reacting isonicotinamide in aqueous
solution with hydrazine at elevated temperatures.
The reaction is preferably effected at a temperature of 1000 C under
reflux.
The reaction proceeds readily in the presence of water and the rate of
reaction and the yield of the hydrazide is influenced by the amount of
water contained in the reaction mixture Relatively large amounts slow
down the reaction and also result in reduced yields of the desired
product It is therefore advantageous to operate in the presence of
sufficient water to produce a homogeneous mixture at the temperature
at D which the reaction is carried out Suitably, a quantity of water
equal to the weight of the isonicotinamide charged can be used or the
amount contained in concentrated commercially available hydrazine
hydrate.
The isonicotinamide used as starting material for the present process

may be obtained from 4-cyanopyridine with good efficiencies by
treating cyanopyridine in an aqueous medium with the oxide, hydroxide
or carbonate of magnesium at elevated temV.
peratures as described in our co-pending Application No 8698/55,
Serial No.
776,313.
Instead of using the isolated isonicotinamide for the process of the
invention, it is 4 possible to use the crude reaction mixture
resulting from the hydrolysis of 4-cyanopyridine, as mentioned above,
and containing besides isonicotinamide, ammonium isonicotinate The
hydrazine is charged 54 advantageously in the form of its hydrate and
it is preferred to use a slight excess, say of 10 %, over the
molecular quantity required by theory.
During the reaction, ammonia is liberated 5 a and the reaction is
complete when the liberation of ammonia ceases.
Isonicotinyl hydrazide is recovered from the reaction mixture by
subjecting the mixture to distillation, preferably under 6 reduced
pressure, whereby water and any free hydrazine are distilled off The
pure hydrazide may be recovered from the solid residue by
crystallisation, for instance from the solution in methanol or ethanol
6 The following examples illustrate the manner in which the process of
the invention is carried out in practice.
EXAMPLE 1.
12.2 parts of isonicotinamide ( 0 1 mole) 7 and 5 parts of 90 %
solution of hydrazine hydrate ( 0 11 mole) were heated under reflux at
1000 C for seven hours, with occasional agitation After this time, the
reaction mixture was distilled at 15 mm Hg 7 to remove excess of
hydrazine The residue, a pale yellow solid, consisted of crude
hydrazide and melted between 1630 and 1660 C.
The yield was 96 5 % based on the isonicotinamide After
crystallisation from 8 C785,346 1785,346 methanol, the pure hydrazide
was obtained in white crystals, m p 171 -173 C Analysis by the method
given in the British Pharmaceutical Codex, 1954, gave a purity of
99-100 %.
When the same Quantities of isonicotinamide and hydrazine hydrate were
heated under reflux with 60 parts of water under otherwise identical
conditions, the hydrazide if was obtained in only 50 % yield based on
the isonicotinamide and its purity was only 82 c.
EXAMPLE 2.
Crude isonicotinamide obtained from hydrolysis of 4-cyanopyridine with
an aqueous suspension of magnesium oxide and containing 88 0 %
isonicotinamide and 3 8 % ammonium isonicotinate was converted to the
hydrazide in the manner shown in 2 ' Example 1 10 parts of the crude
amide and parts of a 90 % aqueous solution of hydrazine hydrate were

heated under reflux with one part of water for eight hours Water and
hydrazine were then removed as before, furnishing a yellow solid, m p
150-163 C, containing 85 % of hydrazide by analysis.
The calculated yield of hydrazide on the amide used was thus 100 %
Crystallisation from methanol furnished a product with a 98 %' purity
and a melting point of 171 ' C.
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* GB785347 (A)
Description: GB785347 (A) ? 1957-10-23
Installation for the dehydration of sludges
PATENT ' SPECIFICATION
m i Date of Application and filing Comp No 19724/55.
Application made in Germany on Aug Complete Specification Published Oc
Index at acceptance: -Classes 23, Pl (A: 1 S); and 34 ( 2), G 2 C 2.
785,347 lete Specification July 7, 1955.
r 17, 1954.
t.23, 1957.
International Classification: -1 BO 4 b F 26 b.
Installation for the Dehydration of Sludges We, VEREINIGTE ALUMINIUM
WERICE AKTIENGESELLSCHAFT, a Body Corporate organised under the Laws
of Germany, of Am Nordbahnhof, Bonn-on-the-Rhine, 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
This invention relates to an installation for the dehydration in

stages of cryolite sludges or similar fine sludges.
In the production of cryolite, cryolite is precipitated from the
aqueous phase, for example by the combination of sodium ana aluminium
salt solutions, possibly with the addition of acids or lyes Only under
certain conditions which cannot always be applied, such as elevated
pressure, is it possible to precipitate the cryolite with a large
grain size in a readily filterable form In general it is not always
possible to work under such conditions, in view of practical
considerations in operation, so that in most processes used at
present, a fine crystalline cryolite sludge is obtained which does not
very readily settle and which is difficult to filter The dehydration
of these fine sludges and, in particular, of those cryolite sludges
which originate from the working up of tar-containing gas scrubbing
lyes from the electrolysis of aluminium, presents great difficulties
At present these lyes, which have a solids content of about 2 to 4 %
are concentrated by sedimentation of the cryolite in large containers
to a content of about 10 % of solids In order to concentrate the
cryolite suspension to this content in a container having a capacity
of cubic metres, however, 4 to 8 days are needed The filtration of
this concentrate also causes further difficulties inasmuch as the
filter cake rapidly becomes impermeable to water and the application
of vacuum or pressure also rapidly terminates filtration It is
therefore possible to work only with very small filter cake layers and
correspondingly large filter surfaces, but even in that case a thick P
1 ice 3 s 6 d l 1 've 4 si 21 sludge still containing 50 to 70 u/, of
moisture, and therefore only 50 to 30 % of solids, is obtained When
working in this way, a large 50 container space is therefore required,
while the dehydration of the cryolite proceeds extremely slowly,
requiring a great deal of manual work and large filter surfaces, and
nevertheless in the end yields a cryolite sludge 55 having a high
water content In addition, a cryolite sludge having this high moisture
content still contains a considerable amount of salts, particularly
sulphates dissolved in the residual lye which then pollute the dried
cryo 60 lite in an undesirable manner and greatly reduce its value
Only by very complicated final washing is it possible when working in
the afore-described manner to reduce the amount of these impurities
contained in the 65 sludge.
The present inevntion provides an installation for the dehydration in
stages of very fine sludge, especially cryolite sludges comprising a
container for the sludge to be dehyd 70 rated, a continuously
operating centrifuge containing a stack of liner plates, means for
conveying concentrated sludge from said centrifuge to a batch
operating centrifuge from which sludge is adapted to be intermittently
75 discharged by means of a knife or scraper, a drying furnace and

means for transferring sludge separated by said batch operating
centrifuge to said drying furnace.
A continuously operating centrifuge having 80 a nozzle outlet and a
sludge worm can advantageously be used in the first stage.
The batch operating centrifuge to be used in the second stage consists
essentially of a drum into which the incoming sludge is intro 85 duced
with the aid of a lateral tube For the purpose of withdrawing the
liquid from this centrifuge use is made of a paring tube and a paring
knife is used to discharge the residue the paring tube and paring
knife being moved 90 along the wall of the drum by means of an oil
hydraulic system A centrifuge having sieve walls can advantageously be
used, that is to say, a centrifuge the drum walls of which consist of
a sieve bed over which a filter cloth is stretched so that a
filtration effect is obtained together with the separation of the
sludge.
If, for example, the starting material is a cryolite sludge containing
2 to 5 % of solids, it is possible to concentrate the centent of
solids in the first stage to about 20 to 3 G%, while after the second
stage solid contents of to 70 %O are obtained Since the amount of
soluble impurities remaining with the isesidual moisture is also
reduced at the same time, it is possible in this way to produce a
substantially purer cryolite, particularly one having a lower sulphate
content.
It has been found particularly advantageous to deliver the sludge
discharged from the batch-operating centrifuge to the drying oven
mechanically by means of a pump, for example a pump known under the
Registered Trade Mark "Mono," This pump consists of a pipe having a
single worm thread, in which a rotor constructed as a two-threaded
worm rotates excentrically.
The sludge is supplied by means of this pump to a drying apparatus,
fox which purpose a rotating drum having simultaneous concurrent flow
and counterfiow firing and sprinkling inserts has given particularly
good results.
It is well known that when cryolite is dried by direct heating, a
certain amount of cryolite is lost with the outgoing gas in the form
of flue dust.
In a further development of the invention, the dust and hydrogen
fluoride passing out with the outgoing gas from the furnace can be
separated and recycled by using a suction fan with the injection of
water or lye, followed by a wet cyclone In the case of high dust
contents in the outgoing gas, previous dry removal of dust, for
example, in a cyclone, has been found convenient.
One embodiment of an arrangement m accordance with the present
invention is illustrated diagrammatically and by way of example in the

accompanying drawing.
Freshly precipitated cryolite sludge 2, having a solid content of
about 3 to 5 %, for example, is contained in a container 1 The
cryolite sludge 2 passes through a pipe 3 and pump 4 to a continuously
operating centrifuge 5 containing a stack of liner plates and which is
indicated only diagrammatically in the drawing The cryolite lye, free
from solids, accruing in the centrifuge 5 is discharged through a pipe
6, while the sludge separated, having a solid content of for example
20 to 30 %, is passed by way of a pipe 7 and pump 8 to a
batch-operating centrifuge 9 from which sludge is intermittently
discharged by means of a knife or scraper When treating sludges having
a uniform concentration of solids, the non-continuous centrifuge 9 can
also be entirely automatically controlled, so that in practice for the
operation of the entire plant, including the drying furnace only one
or two men per shift is or are required with a monthly throughput of
for example 250 tons of cryolite.
In the batch-operating centrifuge, which as shown, has imperforate
walls, three layers 70 are normally found, the cryolite sludge lying
directly on the walis of the drum and having a solid content of about
60 to 70 (% Directly therein lies a turbid lye merging therewithn,
while the clear lye follows in the next layer 75 T 1 he turbid lye can
be drawn off separately and returned through a pipe 10 to the
container 1 The clear lye, on the other hand, is withdrawn through a
pipe 11 The cryolite sludge is discharged by means of a paring 80
knife and delivered to a small bunker 12 which is situated directly in
front of the centrifuge and from which the paste-like cryolite sludge
is pumped to a drying oven 14 by means of a thick sludge pump 13 85
The drying furnace, as previously mentioned, has at its inlet end 15
concurrent flow heating and at its outlet end 16 counterflow heating,
these flows referring to the path of the cryolite sludge The cryolite
discharged 90 at the outlet end 16 contains less than 0 5 % of water
The outgoing gas is drawn off by a blower 18 through a pipe 17 and
subjected to dry removal of dust in a cyclone 19, while the remaining
dust and hydrogen fluoride are 95 recovered by the injection of water
into the blower 18 followed by separation in a wet cyclone 20 This lye
containing solids is returned to the container 1 through a pipe 21.
This mode of operation has the following 100, advantages: 1) The
sludge obtained has a substantially lower water content than hitherto.
2) In the drying of the sludge there can thus be a considerable saving
of heating power 105 3) It is possible to work with a very small
container space.
4) Losses of solids occur neither during the concentration of the
sludge nor during the drying 110 5.) There is a saving of filter
surface, power, and operating labour.

6) The resulting cryolite has a higher degree of purity and in
particular is less contaminated by water-soluble sulphates 115
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