IMPROVEMENTS IN THE MANUFACTURE OF CRYSTALLIZED HYDROCHLORATE OF ALUMINA
Year: 1882

page_text: LETTERS PATENT to William Robert Lake, of the firm of Haseltine, Lake,
& Co., Patent Agents, Southampton Buildings, London, for an invention of
"IMPROVEMENTS IN THE MANUFACTURE OF CRYSTALLIZED HYDROCHLORATE
OF ALUMINA."-A communication from abroad by Thaddéo Gladysz, of
Mailles Transs
PROVISIONAL SPECIFICATION left by the said William Robert Lake at
the Office of the Commissioners of Patents on the 24th April 1882.
WILLIAM ROBERT LAKE of the firm of Haseltine Lake & Co, Patent Agents
"IMPROVEMENTS IN THE MANUFACTURE OF
Southampton Buildings, London
CRYSTALLIZED HYDROCHLORATE OF ALUMINA, [A communication from abroad by
Thaddée Gladysz, of Marseilles, France.]
This Invention relates to the preparation of crystallized hydrochlorate of alumina.
One method by which this is effected according to the said invention, is based
upon the discovery that this compound may be obtained from its solutions by
hydrochloric acid.
In the case of a hydrochloric solution of alumina, oxide of iron, oxide of
manganese, chloride of calcium or other substances (the alumina being predominant)
when hydrochloric gas is introduced into the mixture the hydrochlorate of
alumina after a time commences to be deposited in a perfectly crystallized state.
The precipitation will be complete or nearly complete with the perfect saturation of
the liquid by the hydrochloric gas.
For operating industrially I saturate the solution of hydrochlorate of alumina
obtained either from solution of gelatinous alumina by hydrochloric acid or from
the double decomposition of the alums or sulphates of alumina by chloride of
calcium barium and other substances; I saturate this solution with hydrochloric
gns obtained from any source. As a result I obtain, on the one hand, crystallized
hydrochlorate which when drained and dried in a current of dry air is absolutely
neutral, and on the other hand, the mother liquor of the hydrochlorate, which is
hydrochloric acid retaining all the impurities which accompanied the alumina.

page_text: Hydrochlorate of alumina, thus prepared contains about twenty one per cent of
soluble alumina and about forty four per cent of chlorine.
Another method of preparing crystallized hydrochlorate in accordance with the
said Invention is based upon the discovery that this compound may be concentrated
in aqueous solutions without suffering the least decomposition, provided the
evaporation is effected under a pressure below that of the atmosphere.
For operating industrially I commence by procuring liquid hydrochlorate of
alumina prepared in any well known manner. I prefer the method of preparation
which consists in decomposing sulphate of alumina by chloride of calcium obtained
from soda manufactories. The sulphate of lime obtained in the precipitation is
left well filtered and washed. The liquid hydrochlorate of alumina mixed with
the wash is then concentrated in boilers of tinned copper open to the atmosphere.
This concentration may be carried as far as from 25° to 30° Baumé. At this point
the little sulphate of lime which can be held in solution, is precipitated and may
he lifted from the bottom of the liquid.
The liquid at 25° or 30° Baumé, is then placed in closed boilers of tinned copper
and subjected to concentration. During the heating of the liquid a vacuum is
produced and maintained in the said boiler. The operation of distillation may be
very well effected with a vacuum of fifty or fifty five centimètres of mercury.
The mass may be evaporated until dry or it may be stopped-in-order-to-obtain-a-
slow crystallization and the mother liquor. If the latter method is adopted the
crystals of the hydrochlorate are separated from its mother liquors by drying.
Hydrochlorate of alumina thus obtained may be refined according to the same
process; its composition will be, soluble alumina twenty one per cent, chlorine
-forty-four-per-cent-
The two methods herein before described may be combined in the following
manner that is to say, the crystals of the hydrochlorate are first obtained by
concentration in a vacuum. The mother liquors of the said hydrochlorate
containing all the impurities of the alum-cake-are-then-methodically-saturated_
with hydrochloric gas so as to totally precipitate the remaining hydrochlorate.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed by
the said William Robert Lake in the Great Seal Patent Office on the
24th October 1882.
"
WILLIAM ROBERT LAKE of the firm of Haseltine Lake & Co., Patent Agents,
Southampton Buildings London. IMPROVEMENTS IN THE MANUFACTURE OF
CRYSTALLIZED HYDROCHLORATE OF ALUMINA A communication from abroad by
Thaddée Gladysz, of Marseilles, France.
•
}
This Invention relates to the preparation of crystallized hydrochlorate of
alumina. One method by which this is effected, according to the said invention, is
based upon the discovery that this compound possesses the property of being
separable from its solutions by hydrochloric acid.
In the case of a hydrochloric solution of alumina, oxide of iron, oxide of
manganese, chloride of calcium, or other substances (the alumina being the
predominant substance) when hydrochloric gas is introduced into the mixture the
hydrochlorate of alumina after a time, commences to be deposited in a perfectly
crystallized state. The precipitation will be complete or nearly complete with
the perfect saturation of the liquid by the hydrochloric gas.
For operating industrially I saturate the solution of hydrochlorate of alumina,
(obtained either from solution of gelatinous alumina by hydrochloric acid, or from
the double decomposition of the alums or sulphates of alumina by chloride of
calcium, barium, and other substances) with hydrochloric gas obtained from any
source. As a result I obtain, on the one hand, crystallized bydrochlorate which,
when drained and dried in a current of dry air, is absolutely neutral, and, on the
other hand, the mother liquor of the hydrochlorate, which is hydrochloric acid
retaining all the impurities which accompanied the alumina. Hydrochlorate of
alumina thus prepared contains about twenty one per cent of soluble alumina and
about forty four per cent of chlorine.
Another method of preparing crystallized hydrochlorate, in accordance with the
said invention, is based upon the discovery that this compound can be concentrated
in its aqueous solutions without suffering the least decomposition, provided the
evaporation is effected under a pressure below that of the atmosphere.
For operating industrially I commence by procuring liquid hydrochlorate of
alumina prepared in any well known manner. I prefer the method of preparation
which consists in decomposing sulphate of alumina (alum cake) by chloride of
calcium obtained from soda manufactories. The sulphate of lime obtained in the
precipitation is capable of being easily filtered and washed. The liquid hydro-
chlorate of alumina mixed with the washing water (eaux de lavages) is then
concentrated in boilers of tinned copper open to the atmosphere. This concentration
may be carried as far as from twenty five to thirty degrees Baumé. At this point
the small quantity of sulphate of lime which may be held in solution is
precipitated and can be lifted from the bottom of the liquid.
The liquid at twenty five or thirty degrees Baumé is then placed in closed
boilers of tinned copper and subjected to concentration. During the heating of the
liquid a vacuum is produced and maintained in the said boiler. The operation of
distillation can be very well effected with a vacuum of fifty or fifty five centimetres
of mercury. The mass may be evaporated until dry, or the evaporation may be
stopped in order to obtain a slow crystallization and the mother liquor. If the
latter method is adopted the crystals of the hydrochlorate are separated from its
mother liquors by drying.
Hydrochlorate of alumina thus obtained can be refined according to the same
process; its composition will be soluble alumina, twenty one per cent, chlorine
forty four per cent.

page_text: The two methods herein before described can be combined in the following
manner that is to say the crystals of the hydrochlorate are first obtained by
concentration in a vacuum. The mother liquors of the said hydrochlorate
containing all the impurities of the alum-cake, are then saturated with bydrochloric
gas in order to totally precipitate the remaining hydrochlorate.
Having thus fully described the said invention as communicated to me by my
foreign correspondent and the manner of performing the same I wish it understood
that I claim.
First. The preparation of crystallized hydrochlorate of alumina by the action of
bydrochloric gas in a hydrochloric solution of alumina.
Second. The concentration of hydrochlorate of alumina in aqueous solutions
without decomposition by effecting the evaporation under a lower pressure than
that of the atmosphere.
Third. In carrying my Invention into practice by either of the methods
described the special treatment above set forth.
In witness whereof I the said William Robert Lake have hereunto set my
hand and seal this Twenty fourth day of October in the year of Our Lord
-One-thousand eight hundred and eighty two.