An Improved Method of and Apparatus for Softening Water for Industrial and other Purposes.
Year: 1896

page_text: Date of Application, 6th May, 1896
Complete Specification Left, 6th Mar., 1897-Accepted, 6th May. 1897
PROVISIONAL SPECIFICATION.
An Improved Method of and Apparatus for Softening Water for
Industrial and other Purposes.
We, EMILE D'HUART, of Luxembourg, in the County and State of Luxembourg,
MICHEL GLAESENER, of Chatillon, County of Belgian Luxembourg, Belgium, and
GEORGES GLAESENER, of Chatillon, County of Belgian Luxembourg, Belgium, do
hereby declare the nature of this invention to be as follows:-
The present method has for its object the softening of underground and spring
water for industrial purposes, either for the feed water of steam boilers, or for the
washing of textile fibre and the like, or for any other purpose where the presence of
calcium, magnesium or other hardening matters in the water may be detrimental.
Our invention, in so far as the method is concerned is based upon the following
chemical re-actions:
1. Oleic acid, as a bye-product in the manufacture of stearin, forms with the caustic
alkalies and also with the alkaline carbonates (in the latter case with separation of
carbonic acid) soluble oleates either direct or with the application of a little heat.
2. These alkaline oleates form with soluble calcium, magnesium and other salts
found in the water, light compounds, which being insoluble in water and having a less.
specific gravity rise to the surface of the same, as a doughy material and are easily
separated therefrom.
3. The alkaline oleate compounds also form with aluminium sulphate, ferric sulphate,
alum, ferric alum and similar compounds insoluble oleates of light specific gravity,.
which are readily separated from the water, thus clarifying the water which has
already been freed from the lime, magnesium or other hardening substances.
The application of these reactions to the softening of water may be effectuated in
the following manner :
It is before all necessary to take into consideration the formation of the soluble
alkaline oleates.
I. This is effected by the combined action of oleic acid and alkaline hydrates;
then we proceed as follows: In a suitable water receptacle provided with a stirrer we
introduce into the water to be purified the necessary quantity of oleic acid, and cause
the same by rapid stirring to be held in suspension, a suitable quantity of the solution
of alkaline hydrate being introduced during the movement. In a short time all the
oleates of the hardening elements become separated as insoluble doughy material,
which quickly collects at the surface of the water. The rapidity of separation of this
material may be increased by adding oleic acid. A small excess of alkalies enables
the calcium, magnesium and other hardening salts to be perfectly separated. If the
proper quantity of the alkaline hydrates has been added to the water containing
lime, magnesia, or other hardening matter the water may he used in this state for
industrial purposes if the opalescence of the same has no deleterious effect. It may
however be completely clarified by salts having an acid reaction such as aluminium,
iron or similar acid salts. The alkalinity of the water thus treated may be easily
determined, and a solution of the said salts must be added until it gives a neutral
reaction. The reaction is accelerated by rapid rotary movement. This operation
may be effected in the same receptacle as the first but it may also take place according
to exigencies in a separate receptacle, into which the water passes from the first

page_text: receptacle through a metallic sieve in order that the coarser impurities may be
separated out.
It may also appropriately take place in the presence of frictional
agents, such as sawdust and paper material. Treated in this manner the water passes
into a sand filter which it leaves in a pure state. After its clarification the water must
not contain a trace of the clarifying salts employed. These may be used in a
solid form.
A more troublesome method of clarifying the water from which the hardening matters
have been removed consists in treating this water with small equivalent quantities
of hydrochloric or sulphuric acid. Here, too, there must be a rapid rotary movement
in which the friction may appropriately be increased by clean sawdust or paper
material which is free from lime for the purpose of accelerating the reaction. In this
instance the water-purifying receptacle would require to have a leaden lining. The
filtering material would have to consist of as pure siliceous matter as possible and the
water would have to be finally freed again from the excess of acid by sodium
carbonates or other neutralizing agents.
II. If alkaline carbonates are employed for the formation of the alkaline oleates,
this must be effected by the use of a little heat, say by a current of steam. The
reaction may be effected in the small space which is contained in the water
admission pipe, and into which the appropriate quantities of reagents are brought
together and are intimately mixed say by a current of steam. After the reaction
which scarcely takes a few seconds, the material is conveyed by the water admitted
into the first rotary receptacle in order to be then further treated as above stated.
The alkaline oleate may also suitably be prepared outside the apparatus and being
contained in a suitable vessel, introduced into the water admission pipe.
For the proper progress of the process the proportions of the quantities of reagents
have before all to be considered. No considerable excess of alkaline hydrate or
alkaline carbonate must be employed. The quantity to be used of these bodies must
exactly correspond to the equivalent for the quantity of lime, magnesia or other
hardening matter contained in the water. For determining this equivalent it might
be expedient to ascertain the hardness. But this may suitably be replaced by a new
method which serves as a basis for that of the purification of water. As an example
of the new method forty cubic centimetres of water are mixed with a few drops of
oleic acid in a suitable bottle thoroughly shaken and tenths of normal alkaline liquor
are added until a rapidly vanishing foam is formed. The number of cubic centimetres of
tenths of normal liquor as read off corresponds to the equivalent of the calcium and
magnesium salts. From this the quantities of alkaline hydrates or carbonates to be
used can be calculated for any desired quantity of water. This method permits of an
accurate determination of the hardness of water. Even percentages of lime, magnesia
and other bodies may be most accurately determined by the same. This may further
be advantageously applied to iron, copper and the like and any analytical
determinations may be used in which the substances can be separated as neutral salts,
and in which the metals contained in the latter will combine with oleic acid to
form insoluble compounds.
The oleic acid used in the method herein before set forth may easily be recovered
by treatment of the calcium, magnesium and other oleates with hydrochloric or
sulphuric acid. The water itself whatever may have been its original composition is
brought by the usual reagents to the purity of rain water.
Having thus described that part of our invention which consists of the method, we
shall now proceed to describe that part of our invention which consists of the
apparatus.
In our various experiments we have found that the apparatus hereinafter described
gives the best results.
This apparatus is composed of the following parts:
(a) A spherical receptacle comprising two semi-spherical caps connected along a
diameter by means of bolts with interposition of a packing of indiarubber, asbestos,
felt or any other material ensuring a perfectly tight joint. In the sides of the semi-
apherical caps openings are provided closed by plates of glass or any other transparent

page_text: material adapted to withstand the action of the water and reagents in order to enable
the operator to see the liquid contained in the receptacle and easily follow the
operations.
() Beaters formed of two semicircular segments of different diameters keyed upon
the axis passing by two stuffing boxes through the semispherical caps of the receptacle.
These beaters are set in more or less rapid rotation, according as the operation has to
be conducted with more or less rapidity, by means of a pulley and through the inter-
vention of a belt receiving its movement from any transmitting gear or directly from
the flywheel of the steam engine or the motor in the establishment. Of course the
beaters may also be operated by any other suitable means.
The rotation of the beaters has the effect of energetically whipping the water
contained in the receptacle and thus bringing all the molecules of the water and
reagents more rapidly in contact.
With the object of ensuring the maximum effect we also arrange upon the interior
periphery of the receptacle small projections of flat, cylindrical or any other form; and
in order not to stop the movement of the heater, which would otherwise strike against
these projections, we provide in the semicircular segments notches affording passage
with a minimum amount of play for the projections herein before referred to.
(c) At the upper part of the receptacle are placed the cocks for introducing the
water to be purified and the reagents. At the lower part is placed the discharge cock
and the door for removing the cake formed by the combination of the calcium and
magnesium salts and reagents.
(d) Immediately below the discharge cock we place a filter composed of a receptacle
of cylindrical or other form in which the filtering material (coke, sand, felt, cellulose
or the like) is put. Upon the filtering material is placed a metallic sieve designed to
retain the calcareous cake. This filter may be arranged in such a manner as to cause
it to turn about a horizontal axis facilitating the removal of the said calcareous cake
retained upon the metallic sieve, this cake being caused to drop into a tub or other
receptacle designed to receive it and placed in proximity to the apparatus.
The apparatus thus described may be used for a number of cases when perfect
clearness of the water is not required. When it is desired to completely clarify the
water treated in this apparatus we place immediately below the filter or by the side of
the first apparatus a second spherical receptacle similar to the first except that the
cocks placed at the upper part are replaced by a door adapted to be withdrawn like a
slide or to be opened upon hinges or in any other manner. This door tightly closes
an opening designed for introducing into the spherical receptacle a certain quantity of
sawdust or paper pulp. Through this opening we also admit the purified water coming
directly from the filter herein before described, when the receptacle is placed immediately
below, or through the intervention of a pump when the room at disposal does not
permit of such an arrangement.
Similar beaters to those used in the first receptacle and operated like them whip
again the water brought in contact with the reagents designed to render the water
limpid which leaves the upper receptacle in a more or less opalescent state.
When
this clarification takes place by means of sulphuric or hydrochloric acid the interior of
this receptacle is covered as are also the eaters, discharge cocks and the receptacle
of the filter hereinbefore mentioned with a thin layer of lead in order to protect the
metal from corrosion.
Immediately below this second receptacle is a filter similar to the first; and the
water on leaving this filter is conveyed directly either by pipes or in any other manner
into a cistern, basin or any other receptacle which may be deemed suitable provided
that it is not composed of materials containing calcium or magnesium salts.
Now the mode of operation is as follows:
The first receptacle is connecte.] either to the water supply or to the feed well
through the medium of a pump or a pipe. The water to be purified is introduced into
the receptacle by opening the cock at will and the quantity (say in litres) is indicated
by a water level arranged on the outside of the apparatus and in sight of the operator.
This quantity having entered the apparatus the admission cock is closed and the one

page_text: is opened which admits alkaline hydrate, the quantity of which is determined before-
hand by the degree of hardness of the water to be treated as described in the chemical
description of the process. We close the cock and set the beaters in motion for some
minutes. Then we stop the motion and introduce the desired quantity of fatty acid
whereupon the beaters are again set in motion. We allow them to rotate for some
minutes and then stop them again and we see the calcareous cake completely formed
and floating on the surface of the water. We may also proceed inversely first by
introducing the fatty body and then the alkaline hydrate. After a minute's rest. we
cause the water thus purified to flow out into the filter, which flow lasts for some
minutes. We open the door for removing the cake which falls upon the metallic sieve.
We close it again and also the cock and we introduce a fresh charge of water
recommencing the operation in the same manner. The water leaving the filter if it
is to be rendered absolutely limpid is conveyed into the second receptacle after we
have introduced into the latter a suitable quantity of sawdust and sand, unless we cause
it to flow out directly into the cistern or into the basins designed for its reception after
purification.
When the water has entered the second spherical receptacle we introduce into the
same the desired quantity of the clarifying agent, we close the door set the beaters in
motion and stop them after they have rotated for some minutes. Then we open the
cock which allows it to flow upon the filter whence it leaves in a perfectly limpid state
in order to be conveyed into the storing basins.
All these operations take only about ten minutes and the quantity purified in each
operation depends simply on the capacity of the receptacles.
For example an establishment which requires thirty cubic metres of purified water
per day of twelve working hours may use receptacles having a useful capacity of three
hundred litres which enable three thousand litres to be completely purified per hour
or thirty cubic metres in ten hours.
An Improved Method of and Apparatus for Softening Water for
Industrial and other Purposes.
We, EMILE D'HUART, of Luxembourg, in the County and State of Luxembourg,
MICHEL GLAESENER, of Chatillon, County of Belgian Luxembourg, Belgium, and
GEORGES GLAESENER, of Chatillon, County of Belgian Luxembourg, Belgium, do
hereby declare the nature of this invention, and in what manner the same is to
be performed to be particularly described and ascertained in and by the following
statement :-
The present method has for its object the softening of underground and spring
water for industrial purposes, either for the feed water of steam boilers, or for the
washing of textile fibre and the like, or for any other purpose where the presence of
calcium, magnesium or other hardening matters in the water may be detrimental.
Our invention, in so far as the method is concerned is based upon the following
chemical reactions:
1. Oleic acid, as a bye-product in the manufacture of stearin, forms with the caustic
alkalies and also with the alkaline carbonates (in the latter case with separation of
carbonic acid) soluble oleates either direct or with the application of a little heat.
2. These alkaline oleates form with soluble calcium, magnesium and other salts

page_text: found in the water, light compounds, which being insoluble in water and having a less
specific gravity rise to the surface of the same, as a doughy material and are easily
separated therefrom.
3. The alkaline oleate compounds also form with aluminium sulphate, ferric sulphate,
alum, ferric alum and similar compounds insoluble oleates of light specific gravity,
which are readily separated from the water, thus clarifying the water which has
already been freed from the lime, magnesia or other hardening substances.
The application of these reactions to the softening of water may be effectuated in
the following manner:
It is first of all necessary to take into consideration the formation of the soluble
alkaline oleates.
I. This is effected by the combined action of oleic acid and alkaline hydrates;
then we proceed as follows:-In a suitable water receptacle provided with a stirrer we
introduce in to the water to be purified the necessary quantity of oleic acid, and
cause the same by rapid stirring to he held in suspension, a suitable quantity of the
solution of alkaline hydrate being introduced during the movement. In a short time
all the oleates of the hardening elements become separated as insoluble dougby
material, which quickly collects at the surface of the water. The rapidity of
separation of this material may be increased by adding oleic acid. A small excess of
alkalies enables the calcium, magnesium and other hardening salts to be perfectly
separated. If the proper quantity of the alkaline hydrates has been added to the
water containing lime, magnesia, or other hardening matter the water may be used
in this state for industrial purposes if the opalescence of the same has no deleterious
effect. It may however be completely clarified by salts having an acid reaction such
as aluminium, iron or similar acid salts. The alkalinity of the water thus treated may
be easily determined, and a solution of the said salts must be added until it gives a
neutral reaction. The reaction is accelerated by rapid rotary movement. This
operation may be effected in the same receptacle as the first but it may also take
place according to exigencies in a separate receptacle, into which the water passes
from the first receptacle through a metallic sieve in order that the coarser impurities
may be separated out. It may also appropriately take place in the presence of
frictional agents, such as sawdust and paper material. Treated in this manner the
water passes into a sand filter which it leaves in a pure state. After its clarification
the water must not contain a trace of the clarifying salts employed. These may be
used in a solid form.
A more troublesome method of clarifying the water from which the hardening
matters have been removed consists in treating this water with small equivalent
quantities of hydrochloric or sulphuric acid. Here, too, there must be a rapid rotary
movement in which the friction may appropriately be increased by clean sawdust or
paper material which is free from lime for the purpose of accelerating the reaction.
In this instance the water-purifying receptacle would require to have a leaden lining.
The filtering material would have to consist of as pure siliceous matter as possible
and the water would have to be finally freed again from the excess of acid by sodium
carbonates or other neutralizing agents.
II. If alkaline carbonates are employed for the formation of the alkaline oleates,
this must be effected by the use of a little heat, say by a current of steam. The
reaction may be effected in the small space which is contained in the water admission
pipe, and into which the appropriate quantities of reagents are brought together and
are intimately mixed say by a current of steam. After the reaction which scarcely
takes a few seconds, the material is conveyed by the water admitted into the first
rotary receptacle in order to be then further treated as above stated. The alkaline
olente may also suitably be prepared outside the apparatus, and, being contained in a
suitable vessel, introduced into the water admission pipe.
For the proper progress of the process the proportions of the quantities of reagents
have before all to be considered. No considerable excess of alkaline hydrate or
alkaline carbonate must be employed. The quantity to be used of these bodies must
exactly correspond to the equivalent for the quantity of lime, magnesia or other

page_text: hardening matter contained in the water. For determining this equivalent it might be
expedient to ascertain the hardness. But this may suitably be replaced by a new
method which serves as a basis for that of the purification of water. As an example
of the new method forty cubic centimetres of water are mixed with a few drops of
oleic acid in a suitable bottle thoroughly shaken and tenths of normal alkaline
liquor are added until a rapidly vanishing foam is formed. The number of cubic
centimetres of tenths of normal liquor as read off corresponds to the equivalent of
calcium and magnesium salts. From this the quantities of alkaline hydrates or
carbonates to be used can be calculated for any desired quantity of water.
method permits of an accurate determination of the hardness of water.
percentages of lime, magnesia and other bodies may be most accurately determined
by the same. This may further be advantageously applied to iron, copper and the
like and any analytical determinations may be used in which the substances can be
separated as neutral salts, and in which the metals contained in the latter will
combine with oleic acid to form insoluble compounds.
This
Even
The oleic acid used in the method hereinbefore set forth may easily be recovered by
treatment of the calcium, magnesium and other oleates with hydrochloric or sulphuric
acid. The water itself whatever may have been its original composition is brought by
the usual reagents to the purity of rain water.
Having thus described that part of our invention which consists of the method,
we shall now proceed to describe that part of our invention which consists of the
-apparatus.
In our various experiments we have found that the apparatus hereinafter described
gives the best results.
This apparatus is composed of the following parts:
(a.) A spherical receptacle comprising two hemispherical caps CC connected along
a diameter A B by means of bolts D, with interposition of a packing of indiarubber,
asbestos, felt or any other material ensuring a perfectly tight joint. In the sides of
the hemispherical caps openings are provided closed by plates E of glass or any other
transparent material adapted to withstand the action of the water and reagents, in
order to enable the operator to see the liquid contained in the receptacle and easily
follow the operations.
(b.) Beaters F formed of two semicircular segments of different diameters, keyed
upon the axis G passing by two stuffing boxes H through the hemispherical caps of
the receptacle. These beaters are set in more or less rapid rotation, according as the
operation has to be conducted with more or less rapidity, by means of a pulley I and
through the intervention of a belt receiving its movement from any transmitting gear
or directly from the fly-wheel of the steam engine or the motor in the establishment.
Of course the beaters may also be operated by any other suitable means.
The rotation of the beaters has the effect of energetically whipping the water
contained in the receptacle and thus bringing all the molecules of the water and
reagents more rapidly in contact.
With the object of ensuring the maximum effect we also arrange upon the interior
periphery of the receptacle small projections K of flat, cylindrical or any other form;
and in order not to stop the movement of the beater, which would otherwise strike
against these projections, we provide in the semicircular segments F notches e
affording passage, with a minimum amount of play, for the projections bereinbefore
referred to.
(c.) At the upper part of the receptacle are placed the cocks L for introducing the
water to be purified and the reagents. At the lower part is placed the discharge
cock M and the door N for removing the cake formed by the combination of the
calcium and magnesium salts and reagents.
(d.) Immediately below the discharge cock M we place a filter O composed of a
receptacle of cylindrical or other form, in which the filtering material (coke, sand,
felt, cellulose or the like) is put. Upon the filtering material is placed a metallic
sieve designed to retain the calcareous cake. This filter may be arranged in such a
manner as to cause it to turn about a horizontal axis P facilitating the removal of the

page_text: said calcareous cake retained upon the metallic sieve, this cake being caused to rop
into a tub or other receptacle designed to receive it and placed in proximity to the
apparatus.
The apparatus thus described may be used for a number of cases when perfect
clearness of the water is not required. When it is desired to completely clarify the
water treated in this apparatus we place immediately below the filter O or by the side
of the first apparatus a second spherical receptacle C similar to the first except that
the cocks placed at the upper part are replaced by a door Qadapted to be withdrawn
like a slide or to be opened upon hinges or in any other manner. This door tightly
closes an opening designed for introducing into the spherical receptacle a certain
quantity of sawdust or paper pulp. Through this opening we also admit the purified
water coming directly from the filter hereinbefore described, when the receptacle is.
placed immediately below, or through the intervention of a pump when the room at
disposal does not permit of such an arrangement.
Similar beaters to those used in the first receptacle and operated like them whip
again the water brought in contact with the segments designed to render the water
When
limpid which leaves the upper receptacle in a more or less opalescent state.
this clarification takes place by means of sulphuric or hydrochloric acid the interior of
this receptacle is covered, as are also the beaters, discharge cocks and the receptacle
of the filter hereinafter mentioned, with a thin layer of lead in order to protect the
metal from corrosion.
Immediately below this second receptacle is a filter R similar to the first; and the
water on leaving this filter is conveyed directly, either by pipes or in any other
manner, into a cistern, basin or any other receptacle which may be deemed suitable,
provided that it is not composed of materials containing calcium or magnesium
salts.
Now the mode of operation is as follows:-
We
The first receptacle is connected either to the water supply or to the feed well
through the medium of a pump or a pipe. The water to be purified is introduced into.
the receptacle by opening the cock at will, and the quantity (say in litres) is indicated
by a water level arranged on the outside of the apparatus and in sight of the
operator. This quantity having entered the apparatus the admission cock is closed
and the one is opened which admits alkaline hydrate, the quantity of which is deter-
mined beforehand by the degree of hardness of the water to be treated as described
in the chemical description of the process. We close the cock and set the beaters in
motion for some minutes. Then we stop the motion and introduce the desired
quantity of fatty acid, whereupon the beaters are again set in motion.
allow them to rotate for some minutes and then stop them again and we see the
calcareous cake completely formed and floating on the surface of the water. We may
also proceed inversely, first by introducing the fatty body and then the alkaline
hydrate. After a minute's rest we cause the water thus purified to flow out into the
filter, which flow lasts for some minutes. We open the door for removing the cake.
which falls upon the metallic sieve. We close it again and also the cock, and we
introduce a fresh charge of water, recommencing the operation in the same manner.
The water leaving the filter, if it is to be rendered absolutely limpid, is conveyed into
the second receptacle, after we have previously introduced into the latter a suitable
quantity of sawdust and sand, unless we cause it to flow out directly into the cistern
or into the basins designed for its reception after the purification.
When the water has entered the second spherical receptacle we introduce into the
same the desired quantity of the clarifying agent, we close the door, set the beaters in
motion and stop them after they have rotated for some minutes. Then we open the
cock which allows it to flow upon the filter, whence it leaves in a perfectly limpid state
in order to be conveyed into the storing basins. All these operations take only about
ten minutes and the quantity purified in each operation depends simply on the
capacity of the receptacles.
For example an establishment which requires thirty cubic metres of purified water
per day of twelve working hours may use receptacles having a useful capacity of

page_text: three hundred litres, which enable three thousand litres to be completely purified per
hour, or thirty cubic metres in ten hours.
Having now particularly described and ascertained the nature of our said inven-
tion and in what manner the same is to be performed, we declare that what we
claim is :-
1. The employment of one of the fatty acids, but preferably oleic acid, in com-
bination with alkaline hydrates or alkaline carbonates for softening water containing
lime, magnesia and other ingredients of a hardening nature substantially as set
forth.
2. The method of clarifying the water from which the lime and other hardening
substances have been removed in the manner set forth in the first claim by means of
acids or by acid aluminium, ferric or similar acid salts which form with oleic acid
insoluble compounds, either in the presence, or after the separation, of organo-earthy
lime cake, with subsequent filtration.
3. The arrangement and combination of parts substantially as set forth with
reference to the drawing.
4. The employment of a cylindrical or otherwise shaped receptacle with vanes
or beaters adapted to rotate therein for carrying out the method herein before
described.
Dated this 6th day of March 1897
J. G. LORRAIN,
Norfolk House, Victoria Embankment, London, W.C.,
Chartered Patent Agent.