4706 4710.output

* GB785113 (A)
Description: GB785113 (A) ? 1957-10-23
Improvements in and relating to the treatment of leather diaphragms and the
like
Description of GB785113 (A)
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up-to-date or fit for specific purposes.
PATENT SPECIFICATION
Inventor:-AMBROSE JOHN CRUISE.
Date of filing Complete Specification Dec 20, 1954
Application Date: Sept 22, 1953 N'o 26109/ 53 ' Complete Specification
Published: Oct 23, 1957.
Index at Acceptance:-Classes 2 ( 6), P 8 A, P 8 D( 2 B 2: 8 A), P 8 P(
2 X: 3 6 X), P 9 A, P 9 D( 1 B 1: 3), P 9 P( 2 X: 3: 6 X); and 76, C 2
B. International Classification:-C 14 c.
COMPLETE SPECIFICATION.
Improvements in and relating to the Treatment of Leather Diaphragms
and the like.
We, UNITED GAS INDUSTRIES LIMITED, of 51 Lincoln's Inn Fields, London,
W C 2, a
British Joint-Stock Corporation, do hereby declare the invention, for
which we pray that a patent may be granted to us, and the manner by
which it is to be performed, to be particularly described in and by
the following statement:-
This invention relates to leather diaphragrms and like leather
articles such as are used, for example, in gas meters, gas water
heaters, control devices of various types, pumps, valves and in other
mechanisms or apparatus where the diaphragm or the like is required to

perform an operation in dependence upon the flexibility which it
possesses as a result of the random orientation of the fibres and
fibrils of its structure.
In all such applications of the diaphragm or the like, it is highly
desirable that the initial flexibility of the leather shall be
maintained, to secure uniformity and accuracy in the performance of
the function for which it is used over an extended period.
The flexibility may vary, however, by reason -of the effect of
external influences such as moisture, vapours or gases, or through
changes set up by loss of oil dressing or by absorption of gaseous
constituents or even by reason of repeated flexure mechanically
imposed upon the diaphragm or the like during the performance of-its
function.
The variation in flexibility will be in some instances an increase,
while, in other instances, it will be a reduction, but in all cases
the variation is undesirable.
The invention has among its objects to impart to the leather
diaphragms and the like in question a degree of stability, more f E
particularly in respect of flexibility, greater than that which they
naturally possess, to ensure a higher degree of uniformity and
accuracy of the mechanism in which is used such a diaphragm or the
like, and to lengthen the useful life of such a diaphragm or the like
in the performance of its function.
According to the invention the leather intended for the diaphragms or
the like is treated by impregnation with at least one monomeric
ethylenically unsaturated compound which, applied in an emulsion or
dispersion, polymerises upon the fibres and fibrils of the structure
of the leather.
The monomeric compounds that may be used for the purpose of the
invention include unsaturated polyesters that will polymerise upon and
in the leather treated, to which they may be applied in an aqueous or
oil emulsion or dispersion, or mixtures of compounds which, under like
conditions, will produce copolymers upon and in the leather.
Some of the copolymer-forming compounds that may be used include
acrylonitrile, ethyl meth-acrylate and other suitable compounds that
will polymerise upon a substance immersed in the emulsion or
dispersion in which they are contained These compounds are
polymerisable at room temperatures without additional heat and without
pressure, but the use of heat in a varying degree and pressures
varying from atmospheric pressure is not excluded from the application
of the invention The selection of a particular compound may be
determined according to the degree of stability of the leather
required.
The leather may be submitted to the treatment with the monomeric

polymerisable compound as a distinct step or such treat785 -13 785,113
55.
: 7, 1 1'I 1, e 1 1 785,113 ment may be incorporated with the oil or
other dressings of the leather.
As an example of a specific application of the invention, semi-chrome
leather intended a for the diaphragms of a gas meter, and of a
thickness approximating to 0 5 of a millimetre, is soaked in an
aqueous dispersion of ethyl meth-acrylate of a concentration of about
30 per cent monomer and 70 per cent water for a period ranging from 10
to 30 minutes at room temperature in the range of 550 to 650 F The
leather is then air-dried at a temperature under 1000 F The
methacrylate polymerises into a flexible coating over the fibres and
fibrils of the structure of the leather, and, being flexible, allows
the fibres and fibrils to move freely while restraining any tendency
on their part to contraction.
After drying, the leather is dried and dressed in the usual manner The
effect of the polymerised meth-acrylate on the leather may be
controlled by the concentration of the dispersion in which the leather
is soaked.
It is not essential that the leather shall be soaked in the emulsion
or dispersion For example, the leather may be brushed on one or both
sides over the whole surface or so as to leave an annulus untreated
adjacent the periphery or at the centre, or both Again, the brushing
may be replaced by spraying.
The treatment may take place in the tannery after the fat liquoring,
the emulsion or dispersion being drummed into the leather or skins or
sprayed thereon, in each case before the drying in the tannery.
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* GB785114 (A)
Description: GB785114 (A) ? 1957-10-23

Improvements in luminescent materials
Inventor: PETER WHITTEN RANBY ' Date of filing Complete Specification
Nov 5, 1954.
Application Date Dec 1, 1953.
Complete Specification Published Oct 23, 1957.
Index at Acceptance:-Class 39 (i), 54 (C: F: G: H:-J: P: Q)
International Classification: -C 09 k.
COMPLETE SPECGFICATION Improvements in Luminescent Materials We, THORN
ELECTRICAL INDUSTRIES LIMITED, a British company, of 105-109, Judd
Street, London, W C 1, do hereby declare the inevntion, 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 luminescent materials for
use for example in fluores, cent discharge lamps and in the formation
of cathode ray tube screens and X-ray screens Luminescent materials
comprising calcium pyrophosphate activated by tin have been proposed
in British Patent Specification No.
578,272 The heating conditions disclosed in that specification are
such that the tin compound in the matrix must be in the stannic state
These luminescent materials can be excited by cathode rays but not by
the 2537 or 3650 A U radiations.
Other luminescent materials proposed in our Patent Specification No
746,272 comprise the pyrophosphates of the bivalent metal calcium and
of one or more of the bivalent metals magnesium strontium, barium or
zinc, activated with tin or with both tin and manganese, the
proportion of tin being not less than 005 %' by weight of the
luminescent materials, the composition being such that the molecular
ratio of metal oxide (excluding the tin activator) to phosphorous
pentoxide lies between the limits 2:0 9 and 2:1 4 inclusive, 'and the
amount of calcium constituting not more than 98 molecular per cent of
the total bivalent metal (excluding the tin activator or'the tin and

manganese activators) in the material.
According to the present invention an artificial luminescent material
comprises calcium pyrophosphate, with or without manganese
pyrophosphate, and of the alpha and/or beta form as hereinafter
defined by its X-ray diffraction lines, activated by tin in a lower
valency state than stannic tin, or by tin in the said lower valency
state and the manganese, lPrice 3 s 6 d l the proportion of tin being
not less than 0.05 /' by weight of the luminiescent material, the
composition being such that the molecular -ratio of metal oxide
(excluding the tin acti 50 vator) to phosphorous pentoxide lies
between the limits 2:0 9 and 2:1 4 inclusive, and the manganese when
present constituting up to about one half of: the metal content
(excluding the tin activator) of the luminescent material 55
Preferably the proportion of 'tin is not more -than 10 % by weight
'-of the luminescent material Up to, but not including, 2 molecular
per cent of the calcium may be replaced by one or more of -the metals
strontium, 60 barium, zinc or magnesium.
Materials in accordance with the present invention can be excited to
fluorescence by ultra-violet light of short wavelength, such as the
2537 A U radiation, 65 Also -according to the present invention, a
method of preparing an artificial luminescent material includes the
step of heating at a temperature of above 700 C and below the melting
point of the luminescent material an 70 intimate mixture comprising a
matrix of calcium pyrophosphate, or of calcium pyrophosphate and
magnanese pyrophosphate, or compounds yielding such a-matrix on
heating, and a tin compound in an amount from 0 05 to 75 %', by weight
of the intimate mixture, the composition of the intimate mixture being
such that the molecular ratio of metal oxide (excluding the tin
activator) to phosphorous pentoxide lies between the limits 2:0 9 and
80 2:1 4 inclusive, the heating conditions being such that the tin in
the material is in a lower valency state than stannic tin, and the
calcium pyrophosphate is in the alpha and/or beta form as hereinafter
'defined, and the man 85 ganese compound or compounds, when present in
the intimate mixture, constituting up to about one half of the metal
content (excluding the tin activator) of the matrix.
It is sometimes of advantage to first prepare 90 the calcium
pyrophosphate matrix and then to incorporate the activating tin
compound 785,114 No 33407/53.
r? W, -4,z G rice : 2 785,114 therein by heating unde:iinzoxiidising
or _ The manganese may be added to the inti 45 weakly-reducing
conditions mate mixture in the form of one or more of its Materials
prepared by the method in accor compounds, foir example the carbonate
or dance with the present invention comprise cal phosphate It is at
present believed that at cium pyrophosphate'of the alpha and/or-beta

least some of the manganese incorporated in form as hereinafter
defined the material replaces at least some of the bi 50 Theoretically
the pyrophosphates 'f bi valent -netal present in the matrix.
valent metals contain mnetal 9 ode and phos Suitable mixtures of
compounds yielding phorous pentoxide in the ratio of 2:1 respec the
calcium pyrophosphate matrix on heating tively However a certain
limited latitude in comprise, for example, one or more calcium this
ratio is permitted and the present inven compounds such as the
carbonate, hydroxide 55 tion is concerned only with luminescent etc,
together with the required amount of materials in which the molecular
iatfo lies am-nbiuim -hosphate, or precipitated calcium within the
limits specified above as being pyrophosphate together with calcium
carbonaccording to the present invention It has been ate to make up
the required proportion of calfound that slight changes in the 7 said
moilecul' cium, or together with ammonium phosphate 60 ratio within
the limits spec fie may prqdfce to niake up the required proportion of
phosmarked changes in the colour of the phate, as required
-fluorescence -produced by the -luminescent: The materials of the
present invention are material obtained directly in the form of
powders and The tinmay be-added to the intimate mix it is-not
-necessary to melt or even sinter the 65 ture in the orn of one or
more of its stannous material to obtain luminescence They are
-compounds such as the oxide, chloride and -therefore more suitable
for use in, for example, phosphate, and it is then important that the
-a fluorescent lamp than are materials which heating of the intimate
mixture should be -have been melted or even sintered The carried out
under non-oxidising conditions to fluorescence exhibited by the
materials-when 70 prevent the tin compound or compounds from activated
with tin alone and excited by 2537 undergoing oxidation to the stannic
valency A U radiation is generally blue in colour.
-state Thus, the mixture may be heated in a -When _ manganese is
incorporated the -plugged tube 6 r-a 'covered crucible or in a
fluorescence exhibited is of longer wavelength non-oxidising
atmosphere of, for example, than with tin alone The colour of the 75
steam or nitrogen or mixtures thereof, or mix luminescence is also
dependent, at least to tures of hydrpgen with steamf or nitrogen or
some extent, on the crystal form of the calcium -both The intimate
mixture may be heated in pyrophosphate -matrix, and this in -turn
steam without causing the-formation of oxy depends upon the
temperature of heating.
or hydroxyphosphates becaise the intimate The X-ray diffraction lines
for the form 80 -mixture does not contain a sufficiently high of
calcium pyrophosphate which we have -proportion-of basic metal oxide
for such for called the alpha-form are as follows, where d :mation to

take place If the tin is added to the is the crystal lattice
interplanar spacing in intimate mixture before the heating in the
Angstrom Units and I is the intensity on an form of a stannic compound
or-compounds the drbitrary scale using the terms very strong; 85
atmosphere during the-heat treatment should strong; medium; weak; very
weak (not be such that the compound is reduced to a used):
valency state lower-than stannic tin d I dd I :' 7 04 weak 2 74 medium
182 weak 4 85 weak 2 63 medium 1 77 medium :: 4 18 ':'weak 2 58 medium
1 70 weak 3.72 weak 2 43 medium 160 medium I - 3 49 weak ' 240 medium
1157 weak 3 26 strong 2 08 strong 1 29 medium 315 u'' strong 2 03
medium 1 24 weak 3.04 medium, 1 97 strong Similarly, the X-ray
diffraction lines for the called the beta-form are as follows: form of
calcium pyrophosphate whiih we have': 785,114 d I di I d I 4.72 weak 2
80 medium 2 22 medium 4.43 weak 2 75 medium 1 99 medium 3.34 strong 2
68 weak 1 95 medium 3.22 strong 2 54 medium 1 85 weak 3.09 medium 2 40
weak 1 83 weak 3.01 very strong 2 33 medium 1 77 medium 2.90 medium 2
27 weak 1 31 medium The X-ray diffraction lines have been determined
for the calcium pyrophosphate matrix in the absence of tin and
manganese, the positions and intensities of the lines being only
slightly modified by the incorporation of the tin and manganese The
alpha-form of the calciumrn pyrophosphate is formed at the higher
temperatures up to the melting point and the beta-form at the lower
temperatures; the temperature at which transition from the betato the
alpha-form begins to take place is not precisely known but it is
believed at present to be in the range of about 1100 to 1200 C.
In order to obtain the maximum intensity of fluorescence with
materials predominantly of the beta-form it is desirable that they
should be prepared at temperatures near to the transition temperature.
Methods of preparing luminescent materials in accordance with the
invention will now be described, by way of example All the materials
used should be of the high degree of purity which is recognised in the
art to be necessary.
EXAMPLE 1.
14.0 gins calcium hydrogen phosphate (Ca IPO 4) 0.9 gm diammonium
hydrogen phosphate ((NH 4),HP Oj 0.7 gm stannous chloride (Sn C 12 2
HO) are intimately mixed together and then heated in a current of
steam in a furnace at 1220 C.
for -2 hour When cool the material is ground and can be reheated as
before for another 2 hour When cool the powder shows a blue
flourescence under excitation by 2537 A U.
radiation The material is mainly of the alphaform but may contain a
proportion 'of the beta-form.
EXAMPLE 2.
If the method of Example 1 is modified by including 0 6 gm manganese

hydrogen phosphate (Mn HP 04) in the intimnate mixture and the heating
is carried out in a furnace at 1120 C the product when cool shows a
bright yellow fluorescence under excitation by 2537 A U radiation The
material is essentially of the beta-form.
EXAMPLE 3.
If the method of Example 2 is modified by carrying out the heating at
1220 C instead of 1120 C the product when cool shows a pink
fluorescence under excitation by 2537 A.U radiation.
EXAMPLE 4.
7.0 gins calcium carbonate (Ca CO 3) 10.0 gins diammonium hydrogen
phosphate 65 ((NH,4)HP 04) 0.5 gins stannous chloride (Sn Cl I 2 H O
O) 0.4 manganese hydrogen phosphate (Mn HPO 4) are intimately mixed
together and then heated 70 in a closed silica crucible at 850 C for
hour When cool the product is ground and reheated in -a current of
steam in a furnace at 1220 C The final material is a powder which when
cool shows a pink fluorescence 75 under excitation by 2537 A U
radiation.
The materials of Examples 3 and 4 are of the apha-form but may contain
a proportion of the beta-form If the proportion of the beta-form
becomes appreciable the fluorescence 80 shown is orange due to the
simultaneous emission of pink light from the alphaform and yellow
light from the beta-form In order to obtain as high a proportion of
the alpha-form (pink fluorescence) as possible 85 variations in
temperature during the heating should be avoided (e g by maintaining a
slow steady current of steam) and care should be taken to exclude
impurities which might encourage the formation of the beta-form 90
Patent Specification No 738,490, which was published after the filing
date of the present application, discloses and claims an artificial
luminescent material consisting of one or more of barium phosphate,
strontium phos 95 phate, and calcium phosphate, the material being
activated with tin of which at least part is present in the stannous
state, the composition of the material being such that the ratio of
gram-atoms of metal (excluding the tin 100 activator) to gram-moles of
phosphorous pentoxide is between 2 96: and 2 50:1 inclusive, the
strontium when present without calcium present constituting less than
2 44 gram-atoms of the metal in the material (excluding the tin 105
activator), and the calcium when present constituting less than 0 2
gram-atoms of the metal in the material (excluding the tin activator)
per gram-mole of phosphorous pentoxide.
Such an artificial luminescent material may 110 have an amount of tin
present in the material between 0 01 and 0 08 gram-atoms per grammole
of phosphorous pentoxide.
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* GB785115 (A)
Description: GB785115 (A) ? 1957-10-23
Apparatus for cleaning tanks in ships
7859115 Date of Application and filing Complete Specification
February 1, 1954.
No 2988/54.
Application made in Norway on April 25, 1953.
DO Complete Specification Published: October 23, 1957.
Index at acceptance:-Class 21, C.
Interationaid Classification:-C 121.
COMPLETE SPECIFICATION
Apparatus for Cleaning Tanks in Ships I, AAGE JELMERT, a Norwegian
subject, of Bjrn Farmannsgate 4, Oslo, Norway, 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 statment:The present invention
relates to apparatus for cleaning tanks in ships, which greatly
simplifies the cleaning.
The disadvantages of using sea water for cleaning the tanks in ships
are commonly known and consist mainly in that the walls of the tanks
will corrode as a result of the chemical action of the salts in the
sea water.
Such corrosion will reduce the commercial value of the ship and the
ship may after a lo few years, have to be taken out of service due to
damaged tanks When the tanks in a ship have been cleaned by sea water,
the washing water polluted with mud or dirt is thrown or discharged

overboard The water, containing oil, mud and other impurities,
destroys both animal and plant life along the shores and pollutes the
water in harbours For this reason, most or many harbour authorities
prohibit the cleaning of the tanks in ships whilst the ships are in
harbour and require all ships to clean their tanks while out at sea.
It is obvious that such a method in unnecessarily expensive, in that
it requires extra time and work before the ship can again be loaded or
docked for overhaul.
The advantages obtained in washing and cleaning ships' tanks with
fresh water have long been known, but the difficulties and expense
have been so great that fresh water has not been commonly employed for
this purpose It has been proved uneconomic to buy the large quantities
of fresh water which are required for a thorough cleaning of the
tanks, as the cost of fresh water in many harbours is prohibitive
particularly as the expensive fresh water has to be thrown (Price 3 s
6 d) or discharged overboard together with the mud and other
impurities, as soon as the ship is at sea Furthermore, some ports are
not able to supply the large quantities of fresh water which are
required 50 It is an object of the invention to provide apparatus for
cleaning tanks in ships, by which method a sufficient quantity of
fresh water may be stored and used repeatedly, and by which mud and
other impur 55 ities washed off the walls of the tanks are separated
from the fresh water and are stored in special containers until it is
possible to discharge the mud and dirt at sea.
Thus, the tanks may be cleaned in any 60 harbour without violating any
regulations, as nothing is illegally thrown or discharged overboard,
and the ship is not required to make an unnecessary voyage to sea for
the purpose of cleaning the tanks before it may 65 again be loaded or
docked.
A further advantage of the invention is that the tanks will not be
corroded or will be corroded only to a minor extent if the fresh water
has the desired properties 70 A further feature of the invention
consists in that a detergent may be used together with the fresh
water, thus increasing its cleansing properties Instead of fresh water
a chemical fluid which is suitable for the 75 purpose may be used.
According to the invention apparatus for cleaning a tank in a ship
comprises in combination container means for storing fresh water or
other suitable non-corrosive fluid 80 at one side or end of the tank,
means for pumping the fluid from the storage means to a cleaning
apparatus in the tank, means for pumping the fluid with the impurities
from the bottom of the tank to a settling 85 container provided at the
side or end of the tank remote from the storage means and means for
recycling the fluid from an intermediate position in the settling
container to the storage means 90 2 785,115 According to the invention

furthermore, the storage container and the settling container may be
in open communication and both may be filled, or substantially filled,
with cleaning fluid The invention is diagrammatically illustrated by
way of example in the accompanying drawing, in which a section through
the tanker is shown.
Referring to the drawing, two containers 2 and 3 are disposed one on
each side of an oil tank 1 The containers 2 and 3 are filled with
fresh water or other cleaning fluid, approximately to the level shown
in the drawing The containers 2 and 3 are in communication by means of
a pipe 16, so that when water is withdrawn from one container, the
level of the water in both containers will drop When cleaning the tank
1, the fresh water or other cleaning fluid is pumped by means of a
pump 4 through a pipe 5 to the top of the tank 1 where the cleaning
fluid is passed through a hose 6 to a cleaning apparatus 7 which is
preferably of the Butterworth type.
The cleaning fluid is sprayed against the walls 8 of the tank 1 under
high pressure, and subsequently flows down the walls to the bottom 9
of the tank together with the oil, rust, sand or other material
disengaged from or washed off the walls A powerful pump 10 pumps the
cleaning fluid with the impurities through a pipe 11 and through a
hatch 12 into the upper part of the container 3 The lighter
impurities, such as oil, rise to the surface of the cleaning -fluid,
as indicated at 13, while heavier impurities such as rust, sand or the
like, form a sediment on the bottom of the container 3, as indicated
at 14.
The cleaning fluid is thus separated from the impurities in the
container 3, and the fluid is returned by means of a pump 15, through
the pipe 16 from the container 3 to the container 2, after which the
fluid is recirculated A filter 17 may, if required, be provided in the
pipe line 16.
If the oil 13 at the top of the container 3 is valuable, it may
readily be removed for use or for processing; if not, the oil may be
50 discharged overboard at a suitable time and place when the ship is
at sea.
Near the bottom, the container 3 is provided with a man-hole 18,
through which the heavy impurities 14 may be removed as 55 required.
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* GB785116 (A)
Description: GB785116 (A) ? 1957-10-23
Improvements in and relating to the production of iron catalysts for organic
synthesis
COMPLETE SPECIFICATION
Improvements in and relating to the'Production of Iron
Catalysts for Organic Synthesis
We, COUNCIL FOR SCIENTIFIC AND IN
DUSTRIAL RESEARCH, a corporate body established by Statute, of Charles
House, 5-11,
Regent Street, London, S.W.1, do hereby declare the invention, for
which we pray that patent may be granted to us, and the method by
the following statement:
For the synthesis of hydrocarbon and oxygen-containing compounds
containing more than one carbon atom per molecule from carbon monoxide
and hydrogen, catalysts based on iron as the main ingredient are
particularly suitable.
For use in .a reaction system employing a stationary bed of catalyst
granules or in one in which fine particles of catalyst are maintained
in a fluidtsed bed by the up-flowing stream of reacting gases,
suitable catalysts may be prepared by fusing a mixture of iron oxides
and the oxides or salts of activating metals, or by impregnating a
sintered form of iron oxide with solutions of salts of activating
metals, with or without further sintering of the impregnated material:

Such catalysts possess the merit of cheapness and high resistance to
disintegration, but in order to exhibit activity as catalysts for the
synthesis they usually require reduction in hydrogen for a relatively
prolonged period at a temperature considerably above that normally
employed in the synthesis process (namely, at a temperature within the
range 350" to 500 G.). While these catalysts possess a satisfactory
activity for the synthesis per unit volume of catalyst their activity
per unit weight is low and they tend to favour the production of low
boiling products- and of excessive amounts of gaseous hydrocarbons.
Furthermore, The high density of catalysts prepared in this manner
tends to make them unsuitable for use in a liquid-phase reaction
system where fine particles of catalyst are maintained in suspension
in a liquid medium by the upflowing stream of synthesis gas.
These disadvantages of fused and sintered iron catalysts do not apply
to cataly.sts prepared by precipitation from solutions of the salts of
iron and the activating metals.
Catalysts prepared in this manner are of low density and high activity
per unit weight; they may be brought into a state of high activity by
a short period of treatment in hydrogen at a temperature inthe range
of 280 to 350" C. or by treatment in- carbon-monoxide-containing
gases under conditions similar to those employed in the synthesis
process.
Precipitated catalysts are normally prepared from chemically-pure iron
and the preparation involves the consumption of large quantities of
nitric acid and distilled water. A large and complicated plant is
required for their manufacture. Such catalysts are, therefore, much
more expensive to prepare than the fused or sintered catalysts.
According to the present invention a material reducible to provide a
catalyst for the synthesis of compounds containing more than one
carbon atom per molecule from carbon monoxide and hydrogen is prepared
by heating an intimate mixture of iron oxide with suicient.
alkali-metal carbonate or hydroxide to produce alkali metal ferrite,
decompo.sing the ferrite by treatment with water (when the iron oxide
is liberated in an amorphous and partly hydrated form), washing the
decomposed product with - water until substantially free of alkali
metal hydroxide, re-impregnating the product with 0.1 to 5.0 per cent
of alkali metal salt (such - as the carbonate, and also bringing the
product- to a suitable degree of sub-division. We have found that a
product so prepared requires a reducing or similar pre-treatment only
of the same order as that necessary with precipitated catalysts and
yet has high catalytic activity. The product may be reduced or pre
treated either when prepared or else immedi
mately before use. Under certain circumstances -it may be reduced
under the conditions of the synthesis process in which it is to be

used. The
process does not require the consumption of
expensive chemicals or the use of costly
plant Thus in particular since the ferrite is
washed to remove substantially all the free
alkali metal hydroxide, it is possible to use
relatively inexpensive sodium carbonate or
hydroxide to produce the ferrite and to incor-
porate the more expensive potassium com
pounds in the final product. Even though the
bulk of the alkali metal compound used in the
production of the ferrite is recovered as
hydroxide and can be disposed of as such or
used for the preparation of further ferrite,
there is lesste-apital investment- for - sodium
compounds - than for potassium-compounds
We have also found that impurities in the
original iron oxide such as the oxides of aluminium, silicon,
molybdenum, tungsten, and acidic radicles such as sulphate and
phosphate are converted into water-soluble alkali-metal
salts during the formation of the ferrite and are removed during the
leaching of the product with water. Thus we are able to use cheap
forms of iron oxide so that not only is the process cheap to operate
but it employs cheap raw material.
The intimate mixture of iron oxide and alkali metal carbonate or
hydroxide may be
made by finely powdering the materials. The
mixture may be heated at a temperature within the range 350 to 1,200
C. (the
precise temperature being dependent on the
nature of the iron oxide and the alkali-metal
compound used) for a sufficient length of time to effect a
substantially complete conversion to alkali-metal ferrite. The
sub-division of the
leached product may be by grinding, sizing,
forming, pelleting or the like. The pre-treatment may as usual be by
heating with hydrogen
or carbon monoxide or mixtures of the two to effect partial or
complete reduction of the
iron oxide to metailic iron or to effect partial or complete
conversion to carbides of iron.
Additional promoters may be incorporated by impregnating the washed
iron oxide with a readily decomposable salt of the promoting metal.
Promoters such as copper or silver or other metals which do not form

water-soluble alkali-metal salts under the conditions employed in the
formation of ferrites may be
incorporated in the mixture before it is
heated.
Suitable forms of iron oxide which may be used as raw material for the
preparation of
catalysts according to this invention include
iron ores, iron oxides recovered from the manufacture of -aluminiurir
from: bauxite: steel rolling-mill scale, burnt iron pyrites and
similar naturallg-occurring or- industrial by- -
'product iron oxides.
The invention also includes within its
scope synthesis processes in which the catalyst
is used and the products of such processes.
The -process of preparing the catalyst
according to the invention is illustrated by the
following example, but is in no way restricted
to - the - precise materials and conditions
employedin this example.
EXAMPLE.
@ 1,000 gm. of steel rolling-mill scale, ground
to pass a No. 170 B.S. Test Sieve was
intimately mixed with 860 gm. of powdered anhydrous potassium
carbonate. The mixture was then heated in a muffle furnace at a tem
perature of 1,100 C. for 2 hours. Substan
tially complete conversion of the iron oxide to the double oxide
Fe2O3, K,O was indicated
by the loss in weight accompanying the heat
treatment, and was established by X-ray
diffraction analysis of the resulting product.
The sintered cake was roughly broken and
extracted for 48 hrs., with distilled water in
a continuous extractor of the Soxhlet type.
The dried extracted material (1,100 gm.) con
tained 94.1 per cent by weight or hydrated
iron oxide and 3.9 per cent of potassium salts
calculated as K2O@ and X-ray diffraction
sanalysis indicated--the- absence of potassium
ferrite or crystalline forms of iron oxide. The
main constituent of the aqueous extract was
potassium hydroxide, but the presence of
potassium molybdate and other potassium
salts was also-- established.
The hydrated iron oxide prepared as de

scribed was crushed and graded to form
granules which passed a No. 7 and remained
on a No. 14 B.S. Test Sieve and tested for
activity as a synthesis catalyst in a conven
tional fixed-bed reactor. The density of the
catalyst, the conditions used for the reduction
and the conditions- used and results obtained
in the synthesis are shown in the Table
(catalyst "A"). Results obtained in tests with
two other catalysts, "B," prepared by
impregnating rolling-mill scale with- 2 per
S'ce'n't by weight of- potassium carbonate and
heating to 1,000 C., and "C" prepared by
precipitation with alkali carbonate from solu
tions of ferric nitrate, ferrous chloride and
cupric nitrate - and' addition' of potassium
carbonate to the washed filter cake, are also
shown in the Table. - - -
The data given in this table show that the
bulk density, ease of reduction and activity
for synthesis of Catalyst A, prepared by the
procedure of this invention, resemble those of
Catalyst C, prepared by precipitation, and are
in marked contrast with the properties
possessed by the sintered Catalyst B.
<img class="EMIRef" id="026473826-00030001" />
Catalyst A -B- C
Catalyst bulk density,. g/ml. 0.67 2.00 0.87
Reduction in pure hydrogen
Temperature, C. 350 350 300
Time, hours, for complete
reduction ~ 12.5 46 40
Synthesis
H2.CO ratio of feed gas 2:1 2:1 2:1
Temperature, C. 230 265 230 265 230 265
Pressure, Atm. 20 20 20 20 20 20
Space-velocity of feed
gas l./l. catalyst
space/h. 634 1040 821 1520 810 1454
l./g. catalyst/h. 0.946 1.552 0.411 0.762 0.931
1.671
Carbon monoxide + hydrogen,
converted, per cent 33.5 55.5 32.9 52.7 30.7
50.0

Carbon monoxide + hydrogen,
converted, l./g. catalyst/h. 0.305 0.822 0.128
0.381 0.270 0.789
What we claim is,
1. A method of preparing a material
reducible to provide" a catalyst - for the
synthesis of compounds containing more than
one carbon atom per -molecule from carbon
monoxide and, hydrogen which comprises
heating an intimate mixture of iron, oxide
with sufficient alkali-metal carbonate or
hydroxide to produce alkali metal ferrite, de
composing the ferrite by treatment with water, - washing the
decomposed product, with
water until substantially free of alkali metal
hydroxide, re-impregnating the product with
0.-1 to, 5.0 per cent - of alkali metal salt, and
also bringing the product to a suitable degree
of subdiylsion.
2. A method according to claim 1, wherein
additidnal promoters are incorporated in the mixture before heating.
3.A method according to claim 1 or 2,
wherein additional promoters are incor
porated by impregnating the washed, decom
posed product with a suitable compound of
the promoter.
4. zA- method according to any one of claims 1 -to.3- wherein the
mixture is heated to
a temperature of from 350- to 12000 C
5. A method according to claim 1 of pre
paring a material feducible to provide a
catalyst for the synthesis of compounds con
taining - more than 'one carbon- atom per
molecule from carbon monoxide and hydrogen
substantially as hereinbefore described in the example.
6. A material reducible to provide a catalyst
for the synthesis of compounds containing
more than one carbon atom per molecule from
carbon monoxide and hydrogen whenever prepared according to the
method of any of
claims 1.to 5.
7. A method of preparing a catalyst which
comprises heating a material according to
claim 6 in hydrogen or carbon monoxide or a

mixture thereof.
8. A catalyst for the synthesis of com
pounds containing more than one carbon atom
per molecule from carbon monoxide and hydrogen whenever prepared
according to the
method of claim 7.
9. A process for the synthesis of compounds
containing more than one carbon atom per
molecule from carbon monoxide and hydrogen
in which the synthesis is catalysed with a
catalyst according to claim 8.
10. Compounds containing more than one
carbon atom per molecule whenever produced - by the process claimed in
claim 9.
* GB785117 (A)
Description: GB785117 (A) ? 1957-10-23
Improvements in or relating to fibre-drafting elements
COMPLETE SPECIFICATION Improvements in or relating to Fibre-Drafting
Elements.
We, SILVERTOWN RUBBER COMPANY
LIMITED, (formerly The India-Rubber, Gutta
Percha & Telegraph Works Company
Limited), a British Company, of Herga House,
Vincent Square, London, S.W. 1, and

WILLIAM HENRY MARTIN, a British Subject, of the Company's address -at
Silvertown
Works, Silvertown, London, E.16, do hereby declare the invention, for
which we pray that a patent may be granted to us, and the method by
the following statement:
The invention relates to fibre-drafting elements used in connection
with the manipulation of fibres of cotton,. rayon, wool, glass,
asbestos and the like, such elements com prising spinning roll cots,
textile roll covers and draft aprons and other elements used in
various operations connected with spinning.
A spinning roll cot or textile roll cover is, or may be, mounted on a
metal roller or spindle rotating in opposed relation to a fluted metal
roller. The textile fibres are passed through the opposed rollers and
are drawn therefrom into engagement with a further similar pair of
opposed rollers or like means of drafting rotating at a higher speed.
A draft apron, which is an endless belt or band, is, in one
arrangement mounted on and rotates with a pair of metal rollers in
opposed relation to a similar apron mounted in the same way. Between.
the aprons. the textile fibres are supported and nipped in their
passage towards a pair of drafting rollers rotating at a greater
surface speed than the draft aprons.
Other arrangements of draft aprons are used.
Natural rubber is not suited for fibre drafting elements for use with
fibres -. containing natural oils or which are wetted prior to spin-
ning with spinning oils because of the adverse effect of the oils on
the rubber and such elements have, in recent years, been manufactured
from oil resistant synthetic rubbers such as butadiene/acrylonitrile
copolymers as sold under the Registered Trade Marks " Polysar ",
"Hycar", "Paracril", "Chemigum", and Perbunan", and polymerized
chloroprene (neoprene). - A disadvantage d synthetic rubbers for this
purpose is that the textile fibres have an undue tendency to "lapping"
round the fibredrafting elements. "Lapping" means that the fibres
instead of passing through the fibre-drafting elements, cling to and
go round with these elements causing breakage, thinning out or general
unevenness of the thread, or the building upon the fibre-drafting
elements of bunches of fibre which are eventually carried along with
the thread and produce hard and/or soft places and slubs in the
finished yarn.
There are several causes of lapping. We believe that one of these is
connected or related to electrostatic phenomena. Whilst this has not
so far as -we are aware, been conclusively proved, we are satisfied
that the electrostatic properties o a drafting element are important
and that electrostatic attraction may at least aggravate lapping. In

use the rubber becomes charged with static electricity asZ a result of
friction with the fibres and on. account of the high resistivity of
the rubber the charge may reach a comparatively high value and be very
difficult to discharge. Accordingly, the rubber wiU develop a
substantial attraction for the fibres which it is difficult to remove.
Many proposals have been. made for reducing lapping with synthetic
rubber drafting elements. These proposals include the addition of
various substances to the synthetic rubber, such as electrolytes which
are readily soluble in water (e.g. calcium! nitrate) and which effect
the -electrical propertiesof the material The function of such an
added soluble electrolyte is dependent upon the presence of water
(e.g.
absorbed from the atmosphere or applied by dipping the rubber article
into water) and the difficulty arises that as the electrolyte is
soluble in the water, it is gradually leached out of the rubber and in
time loses some of its efficacy.
According to the present invention a fibre
drafting element composed of a vulcanised butadiene/acrylonitrile -
copolymer or polymerised chioroprene synthetic rubber is rendered
water absorbent and hence less prone to the accumulation
of-electrostatic charges. likely to cause lapping, by the addition tot
the rubber
of one or more water insoluble hydrophilic - inorganic materials, such
as precipitated sili
cates and oxides and bentonite clay.
The term "hydrophilic" is used herein to
mean "water attracting" as distinct from
"water retentive ". Thus the hydrophilic
materials used in the invention have the pro
perty of attracting moisture from the atmo
sphere which ensures continuously sufficient
electrical conductivity inthe drafting elements
to permit dissipation of electrostatic charges;
The addition of substances such as diatoma
ceous earth which are merely capable of retain
ing large quantities of water does not ensure
continued conductivity because the water may
dry out, in time,
Materials which may be used include, for
example, precipitated aluninium silicate, pre
cipitated calcium silicate, precipitated
aluminium oxide, activated alumina, as well as
bentonite clay. ~
The materials may be added (e.g. as fillers)

in proportions of 100-150 or more parts by
weight of the material to 100 parts of the syn
thetic rubber. For exampIe when one of the
silicates is used alone it may be added in proportion of 100 parts to
100 parts of rubber and
when a mixture of a silicate and bentonite clay
is used these may be 30-75 parts of the
silicate and 30-75 parts of the clay to each
100 parts of rubber. A water absorption up to
a maximum of 40-45% by volume of the
composition is desirable.
A further difficulty which arises with draft-
ing elements. the synthetic rubber. used in
the invention is that although the rubber is
oil resistant, nevertheless the natural oils in
the fibres and oils added to assist the spinning
operation are found to cause local swelling of
the elements where they are in substantial con
tact with the fibres. Some tackiness of the sur
face of the elements may also be caused but
this largely can be overcome by choice of suit
able plasticisers. An advantage of the addition
of the hydrophilic materials according to the
invention is that they cause an overall swelling
of the -element in which is greater than, and
substantially masks, the local swelling caused
by the~oils.
The following are specific examples of com-
positions suitable for drafting elements:
FIRST COMPOSITION
(Particularly suitable for synthetic fibres).
Shore durometer (type A) hardness 80-84
Colour grey
Sp. Gr. 1.40
Test-cure 30 means. at 310 F.
Polysar (Registered Trade Marl)
N.P. 350 (butadiene/acryloni-
trile rubber) - - - - 34.2%
Vulcanised oil - - - - 3.5%
Stearic acid - - - - - 0.2%
Pale cumarone indene resin ~ - 2.7%
Pale cumarone resin liquid - - 3.0%
Agerite (Registered Trade Mark)
powder - - - - - 0.4%

Resin oil - - - - - - 1.4%
Titanium dioxide 98% - 3.6%
Graphite - - - - - 1.8%
Bentonite clay - - - - - 24.8%
White A.R.F. (prepared
aluminium silicate) - - - 20.0%
Santomerse D (Registered Trade Mark) - - - - - 0.5% - Zinc oxide - --
- - 1.8%
Ground sulphur - - - - 1.4%
Altax (Registered Trade Mark) accelerator - - - - - 0.7% 100.0%
SECOND COMPOSITION
(Particularly suitable for natural fibres-e.g.
~wool and cotton).
Shore durometer hardness 80-84
Colour grey
Sp.- Gr. 1.30 -
Test cure 10 mins. at 310 F.
Polysar (Registered Trade Mark)
N.P. 350 (butadiene/acryloni-,
trile rubber)
Pale cumarone resin -
Resin oil - - - - - - 2.0%
Agerite (Registered Trade Mark)
powder - - - - - 0.7%
Titanium dioxide 98% - - - 3.5%
Graphite - - - - - - 2.0% Bentonite- clay - - - - 17.03 %
White A.R.F. (prepared aluminium silicate) - - - 12.1%
Ground glass 100 mesh - - 22.0%
Zinc oxide - - - - - 2.2%
Ground sulphur - - - - 0.07%
Tuads (Registered Trade Mark) accelerator - - -- - 1.4%
- -- 100.00%
In the above compositions. the bentonite clay
and the aluminium silicate are the water in
soluble hydrophilic inorganic materials
employed in accordance with the invention.
Each of the above compositions is
thoroughly and evenly mixed in a mixing mill
and processed according to normal procedure.
For spinning cots and textile roll covers the
composition is extruded, vulcanised and cut to
length. For draft aprons a layer of the compo-
sition is wrapped on a cylindrical mandrel and
a textile reinforcement wound on, after which

a further layer of composition is applied and
the whole is vulcanised.
It has been found that even with fibre draft
ing elements incorporating hydrophilic
materials according to the invention, initial
lapping difficulties are sometimes experienced
when the elements are first used in a mill. A
certain time interval seems to occur before the
element absorbs - a sufficiency of water, and
during this time interval the textile fibres lap up. With a view to
reducing this difficulty there is, in a preferred form of the
invention, incorporated in the synthetic rubber mixture, a wetting
agent. Examples of suitable wetting agents are the sulphonated lorol
types, such as Facemol (Registered Trade Mark) and the alkyl aryl
types such as Santomerse D (Registered Trade Mark) embodied in the
first of the above examples. The wetting agent decreases surface
tension and as a result imparts to the fibre drafting element the
property of more rapid water absorption. Such wetting agents are water
soluble and may be gradually leached out of the fibre drafting
element, but before this can occur the wetting agent is no longer
required, since the fibre drafting element has absorbed a sufficiency
of water through the presence of the hydrophilic inorganic filler, as
already explained. The wetting agent is used solely to accelerate the
initial intake of water.
What we claim is : -
1. A fibre-drafting element composed of a vulcanised
butadiene/acrylonitrile copolymer or polymerized chloroprene synthetic
rubber and rendered water absorbent and hence less prone to the
accumulation of electrostatic charges likely to cause lapping, by the
addition to the rubber of one or more water insoluble hydrophilic
inorganic materials, such as precipitated silicates and oxides and -
bentonite clay.
2. A fibre-drafting element as claimed in
Claim 1 in which the hydrophilic material comprises precipitated
aluminium silicate.
calcium silicate.
aluminium oxide.
Claim 1 in which the hydrophilic material comprises activated alumina.
6. A fibre-drafting element as claimed in any one of rhe preceding

claims in which the hydrophilic material (or the mixture thereof) is
added in proportion of 100 or more parts by weight of the material or
mixture to 100 parts of the synthetic rubber.
Claim 6 in which the proportion of hydrophilic material is less than
150 parts to 100 parts of synthetic rubber.
8. A fibre-drafting element as claimed in any one of the preceding
claims having a water absorption of 4O-45 % by volume of the com
position.
9. A fibre-drafting element as claimed in any one of the preceding
claims and including a wetting agent.
10. A fibre-drafting element having a composition substantially
according to either of the foregoing examples.
PROVISIONAL SPECIFICATION
Improvements; in or relating to Fibre-Drafting Elements
We, THE INDIA-RUBBER, GUTTA PERCHA &
TELEGRAPH WORKS COMPANY LIMITED a
British Company, of Herga House, Vincent
Square, London, S.W.1, and WILLIAM HENRY
MARTIN, a British Subject, of the Company's address at Silvertown
Works, Silvertown, London, E.16, do hereby declare this invention to
be described in the following statement:
The invention relates to fibre-drafting elements used in connection
with the manipulation of fibres of cotton, rayon, wool, glass,
asbestos and the like, such elements com6 prising spinning roll cots,
textile roll covers and draft aprons and other elements used in
preparing the fibres for spinning.
A spinning roll cot or textile roll cover is mounted on a metal roller
or spindle rotating in opposed relation to a fluted metal roller. The
textile fibres are passed through the opposed rollers and are drawn
therefrom into engagement with a further similar pair of opposed
rollers rotating at a higher speed.
A draft apron, which is an endless belt or band, is, in one
arrangement mounted on and rotates with, a pair of metal rollers in
opposed relation to a similar apron mounted in the same way. Between
the aprons the textile fibres are supported and nipped in their
passage towards a pair of drafting rollers rotating at a greater
surface speed than the draft aprons.
Other arrangements of draft aprons are used.
Natural rubber is not suited for fibre drafting elements for use with
fibres containing natural oils or which are wetted prior to spinning
with spinning oils because of the adverse effect of the oils on the
rubber and such elements have, in recent years, been manufactured from
oil resistant synthetic rubbers such as butadienelacrylonitrile

copolymers as sold under the Registered Trade Marks " Polysax".
"Hycar", "Paracril", " Chemigum ", and " Perbunan ", and polymerized
chioroprene (neoprene). A disadvantage of synthetic rubbers for this
purpose isthatthe textile fibres' have an undue tendency to "lapping"
round the fibre-drafting elements. " Lapping " means that the fibres
instead of passing through the fibre-drafting elements, cling to and
go round with these elements causing breakage, thinning out or general
unevenness of the thread, or the building up; on the fibre-drafting
element of bunches of fibre which are eventually carried along with
the thread and produce hard and/ or soft places and slubs in the
finished yarn.

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