Improvements in the Manufacture of Cement.
Year: 1897

page_text: PROVISIONAL SPECIFICATION,
Improvements in the Manufacture of Cement.
We, CHARLES EUGENE LEE, of 275, Water Street, New York City, State of New
York, U.S.A., temporarily residing in Norfolk Street, Strand, in the County of
London, Electrical Engineer, and CHARLES FRANCIS L'AWTON, of Water Street,
New York City, aforesaid, Chemist, do hereby declare the nature of this invention
to be as follows:-
This invention relates to cements for cementing one article to another, by means
of the use of sodium tetra silicate as a basis for adding other valuable ingredients
for the purpose of making a material which is capable of being and is primarily
plastic in its nature, and afterward, by the addition of other ingredients, becomes
hard, adhesive and anhydrous and incapable of absorbing water or gases, which
with most other cements render such materials liable to deteriorate by time. We
Siso accomplish the perfection of our cement, to make it permanently anhydrous
and hard, by the use of a very moderate degree of heat, not over 300°, and is sub-
jected to this low temperature for a period of not over 5 or 6 hours. We are aware
that silicate of soda has heretofore been used as a basis for cement more or less
hard and anhydrous, in various ways. Therefore we do not claim broadly such a
cement, but the present invention is confined to substantially the chemical con-
stituents hereinafter set forth in this specification, and the method of compounding
the same.
In order that persons skilled in the art to which this invention appertains, may
understand clearly, how to compound and use the invention, we will proceed to
describe it as follows:-
To begin with, we prepare a sodium-tetrasilicate Na, Si, O, by fusing together
180 parts of white sand or powdered quartz, 100 of calcined soda ash and 3 parts
of charcoal, all in powder and intimately mixed. After cooling, the hard mass so
produced is reduced to fine powder and boiled in water, which dissolves it to a trans-
parent syrupy fluid, containing such a proportion of water to the solid matter, in
solution if the right quantity of water and tetrasilicate is used that the latter shall
form from fifteen to twenty per cent. of the whole solution. Then to 3 gallons of
the above solution containing say 17 per cent. of sodium tetra silicate, we add 3
pounds of finely powdered calcium carbonate, 12 pounds of very finely ground
quartz and 3 pounds of a fine ground compound made by fusing in a crucible or on
the hearth of a reverberatory furnace an intimate mixture of 60 parts quartz sand,
28 lime, 34 parts alumina and five calcined carbonate of soda. If silicate of
alumina is used in place of alumina, then the quantity of this silicate should be
increased and the quartz sand diminished so as to keep the relative proportions of
alumina and silica as above stated. After thorough fusion, the mass is cooled,
broken up and ground to fine powder.

page_text: After the foregoing ingredients are mixed and ground together, one pound of
anhydrous antimonic oxide Sb. O, is ground fine with ten ounces of water and then
added with most thorough stirring or mixing to the first mixture above described,
and the cement will be all the better if the whole compound is ground through a
paint mill, set for fine grinding, the result will be a thick, smooth, pasty liquid,
having a slightly grayish white color, and will be then ready for use for cementing
sand, gravel or other substances on to the backs of glass or other tiles, or for cement-
ing sand, gravel or crushed stone on to the faces of bricks or for putting a smooth
white hard finish on the faces of the same. When desired, colours or tints may be
added to the cement before it is ground through the paint mill, so as to give the
faces of the brick any tint wanted, and where transparent glass is used for the
tiles, the color of the cement showing through the glass will give the tiles any
color wished for. Where an even surface is wanted on rough or badly moulded
bricks, the cement is better when thickened by addition of fine sand, ground quartz
or carbonate of lime in fine powder in quantity according to the material used for
thickening and the condition of the bricks used for facing.
The fused silicate of lime, alumina and soda which enters into the composition
of the cement, may be varied somewhat from the proportions above given, and
yet make good cement, and when a darker color is not objectionable, I have obtained
excellent results by substituting iron oxide for one half or more of the lime in the
compound fused. The addition of the iron oxide makes the mixture more easily fused
and also has greater effect in making the finished.cement become insoluble after it
is applied.
It is necessary to use the antimonic oxide in the anhydrous state, Sb. O, for if
the hydrated acids H Sb O, or H, Sb. O, are used, they will set the liquid cement
at once as soon as added into a solid unworkable mass. The anhydrous antimonic
oxide however, after mixing with the other ingredients very slowly, or quickly if
the cement is heated, becomes hydrated and then attacks the carbonate of lime
present, producing insoluble calcium antimoniate and setting free carbon dioxide,
which carbon dioxide combining with the soda produces insolubility in the alkaline
silicate present. This action appears to take place even after the cement has dried
to that degree that it is as hard as glass, for notwithstanding its hardness, the cement
contains from ten to fifteen per cent. of water which appears to be chemically,
though somewhat loosely combined with the alkaline silicate.
The addition of the fused and fine ground silicate of alumina lime and soda or
silicate and aluminate of lime, soda and iron contributes to the hardness and
insolubility of the cement and also prevents blistering or frothing of the hard dried
cement when it is strongly heated, and prevents effloresence of carbonate of soda
on the surface, in the lapse of time. The applicants will not undertake to say
what are the chemical reasons for this action of the fused and powdered compound 4
silicate, but a good deal of experience with the substance has clearly demonstrated
its value for the purpose described.
There are some naturally occurring compound silicates analogous to the above
described artificial compound, which can be used with nearly equal effect in place
of the artificial, as prehenite, epidote, ferruginous hornblende (particularly those 4
kinds containing alumina); jadeite, augite, pyroxine and those eruptive rocks
rich in some of these minerals, also cinders of analogous composition produced in
the manufacture of pig iron from certain kinds of ore.
After the cement is applied and becomes dry it is exceedingly hard, but is also
too easily affected by prolonged soaking in water, unless the cement coated articles 5
have been allowed to stand a long time before immersing in the water, in which
case, i.e. by long standing, chemical changes slowly change the character of the
compound which ultimately becomes totally unaffected by any amount of exposure
to water. To hasten this change, which produces perfect insolubility, after the
articles are coated or cemented and become hard by drying in air, they are placed 5
in an oven and slowly heated up to a temperature of 220° to 235° Fah., and main-
tained at this heat for from one to five hours according to the nature of the articles,

page_text: bricks faced with glass requiring a much longer time than glass or porcelain tiles
coated with a rough backing.
Dated this 19th day of October 1897.
Improvements in the Manufacture of Cement.
We, CHARLES EUGENE LEE, of 27. Water Street, New York City, State of New
York, U.S.A., temporarily residing in Norfolk Street, Strand, in the County of
London, Electrical Engineer, and CHARLES FRANCIS LAWTON, of Water Street,
New York City, aforesaid, Chemist, 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:-
This invention relates to an improved manufacture of cements by means of the
use as a basis of sodium tetrasilicate to which are added other valuable ingredients
for the purpose of making a material that is capable of being and is primarily
plastic in its nature, and afterward, by the addition of other ingredients, becomes
hard, adhesive and anhydrous and incapable of absorbing water or gases, which
render most other cements liable to deteriorate after a time. We also increase the
efficiency of our cement, in making it permanently anhydrous and hard, by the use
of a moderate degree of heat, not higher than 300° F., the materials being sub-
jected to this low temperature for a period of not more than 5 or 6 hours. We are
aware that silicate of soda has heretofore been used as a basis for cement that is
more or less hard and anhydrous, in various ways. We therefore do not claim
broadly such a cement, but the present invention is confined to substantially the
chemical constituents hereinafter set forth in this specification and the method of
compounding them.
In order that persons skilled in the art to which this invention appertains may
understand clearly how to compound and use the cement according to this inven-
tion, we will proceed to describe it, as follows:-
We first prepare sodium-tetrasilicate Na, Si, O, by fusing together 180 parts of
white sand or powdered quartz, 100 of calcined soda-ash and 3 parts of charcoal,
all in the state of powder and intimately mixed. After cooling, the hard mass
thus produced is reduced to fine powder and boiled in water, which dissolves it to
a transparent syrupy fluid containing such a proportion of water to the solid matter,
in solution if the right quantity of water and tetrasilicate is used, that the latter
shall form from fifteen to twenty per cent. of the whole solution. Then to 3 gallons
of the above solution containing say 17 per cent. of sodium tetrasilicate we add
3 pounds of finely powdered calcium carbonate; 12 pounds of very finely ground
quartz and 3 pounds of a finely ground compound made by fusing in a crucible or
on the hearth of a reverberatory furnace an intimate mixture of 60 parts quartz
sand, 28 parts lime, 34 parts alumina and five parts calcined carbonate of soda
these proportions being by weight. If silicate of alumina is used in place of
alumina, then the quantity of this silicate should be increased and the quartz sand
diminished so as to maintain the relative proportions of alumina and silica as
above stated. After thorough fusion, the mass is cooled, broken up, and ground
to.fine powder.
After the foregoing ingredients are mixed together and ground, one pound of.
anhydrous antimonic oxide Sb. O, is ground fine with ten ounces of water and then

page_text: added to and thoroughly stirred or mixed with the first mixture above described,
and the cement will be improved if the whole compound is ground in a paint mill,
set for fine grinding. The result will be a thick, smooth, pasty mass, having a
slightly grayish white color, and will be then ready for use for cementing sand,
gravel or other substances on to the backs of glass or other tiles, or for cementing
sand, gravel or crushed stone on to the faces of bricks or for putting a smooth white
hard finish on the faces of the same. When desired, colors or tints may be added
to the cement before it is ground through the paint mill, so as to give the faces of
the brick any desired tint wanted, and, where transparent glass is used for the
tiles, the color of the cement showing through the glass will give the tiles any
color wished for. Where an even surface is desired on rough or badly moulded
bricks, the cement is better when thickened by the addition of fine sand, ground
quartz or carbonate of lime in fine powder in suitable quantity which may vary
according to the material used for thickening and the condition of the bricks used
for facing.
The fused silicate of lime, alumina and soda which enters into the composition
of the cement, may be varied somewhat from the proportions above given, and yet
make good cement, and when a darker color is not objectionable, we have obtained
excellent results by substituting iron oxide for one half or more of the lime in the
fused compound. The addition of the iron oxide enables the mixture to be more
easily fused and also has the effect of making the finished cement become insoluble
after it is applied.
It is necessary to use the antimonic oxide in the anhydrous state, Sb. O, for if
the hydrated acids H Sb Q, or H. Sb. O, are used, they will set the liquid cement at
once into a solid unworkable mass. The anhydrous antimonic oxide however,
after mixing with the other ingredients very slowly, or quickly if the cement be
heated, becomes hydrated and then attacks the carbonate of lime present, producing
insoluble calcium antimoniate and setting free carbon dioxide, which carbon dioxide
combining with the soda produces insolubility in the alkaline silicate present. This
action appears to continue even after the cement has dried to that degree that it is
as hard as glass, for notwithstanding its hardness, the cement contains from ten to
fifteen per cent. of water which appears to be chemically, though somewhat loosely
combined with the alkaline silicate.
The addition of the fused and finely ground silicate of alumina lime and soda
or silicate and aluminate of lime, soda and iron contributes to the hardness and
insolubility of the cement and also prevents blistering or frothing of the hard dried
cement when it is strongly heated, and prevents effloresence of carbonate of soda
on the surface after a lapse of time. We do not undertake to say what are the
chemical causes of this action of the fused and powdered compound silicate, but
considerable experience with the substance has clearly demonstrated its value for
the purpose described.
There are some naturally occurring compound silicates analogous to the above
described artificial compound, which can be used with nearly equal effect in place
of the artificial, as prehnite, epidote, ferruginous hornblende (particularly those
kinds containing alumina); iadeite, augite, pyroxine and those eruptive rocks
which are rich in some of these minerals, also cinders of analogous composition
produced in the manufacture of pig iron from certain kinds of ore.
After the cement is applied and becomes dry it is exceedingly hard, but is also
easily affected by prolonged soaking in water, unless the cement coated articles
have been allowed to stand a long time before immersing in the water, in which
case, i.c., by long standing, chemical action slowly changes the character of the
compound which ultimately becomes practically unaffected by exposure to water.
To hasten this change, which produces practically perfect insolubility, after the
articles are coated or cemented and become hard by drying in air, they are placed
in an oven and slowly heated up to a temperature of 220° to 235° Fah., and main-
tained at this heat for from one to five hours according to the nature of the articles,

page_text: bricks faced with glass requiring a much longer time than glass or porcelain tiles
coated with a rough backing.
Having now particularly, described and ascertained the nature of the said
invention and in what manner the same is to be performed we declare that what
we claim is :-
The herein described composition of matter consisting of tetrasilicate of sodium,
with calcium carbonate, powdered quartz, silicate and aluminate of lime and soda
or silicate and aluminate of lime, soda, and iron, and anhydrous antimonic oxide all
compounded and treated substantially as and for the purpose described.
Dated this 18th day of March 1898.