IMPROVEMENTS IN AND RELATING TO THE MANUFACTURE OF GRAPE- " SUGAR
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 AND RELATING TO THE MANUFACTURE OF GRAPE-
"
SUGAR"
A communication from abroad by Doctor Arnot Behr of Jersey
PROVISIONAL SPECIFICATION left by the said William Robert Lake at the
Office of the Commissioners of Patents on the 4th January 1882.
WILLIAM ROBERT LAKE of the Firm of Haseltine Lake and Co., Patent Agents,
Southampton Buildings London "IMPROVEMENTS IN AND RELATING TO THE
MANUFACTURE OF GRAPE-SUGAR [A communication from abroad by Doctor
Arnot Behr of Jersey City New Jersey United States of America Chemist.]
"
Crystallized grape-sugar, as heretofore produced from a watery solution, consists
of the hydrate of grape-sugar containing in its pure state 9.09 per cent of water in
chemical combination. This water is called "water of crystallization." The
crystallized hydrate of grape-sugar loses this water of crystallization if exposed to
a temperature of from 160° to 212° Fahrenheit. In form the crystallized hydrato
is composed of spherical aggregations of minute tablets.
It has been known that crystallized anhydrous grape-sugar may be produced by
dissolving grape-sugar in strong alcohol and crystallizing it from this solution.
Anhydrous grape-sugar is distinguishable from the hydrate, first by its crystalline
form, which is that of needles or prisins, and secondly by the absence of water of
crystallization. When the anhydride is pure, if it be exposed to a temperature of
from 160° to 212° Fahrenheit, it will not lose in weight, while, as has been
observed, the hydrate, under similar circumstances, loses about nine per cent of its
weight.
It is one object of my Invention to produce crystallized anhydrous grape-sugar,
or in other words, crystallized anhydride of grape-sugar, from a watery solution.
The first part of my Invention consists in forming a watery solution of ordinary
commercial grape-sugar, containing not more than fifteen per cent of water.
This

page_text: solution is prepared at, or heated to, a temperature of from 140° to 180° Fahrenheit,
and there is stirred into it a minute quantity, say one hundredth of one per cent,
of previously prepared finely divided anhydride of grape-sugar. The hot mass is
then deposited in moulds, in which it may be allowed to rapidly cool down to about
100° Fahrenheit, from which point it is slowly cooled to about 85° Fahrenheit, the
time occupied in the slow cooling being from two to three days or until the
contents of the moulds are thoroughly crystallised. The object of the slow cooling
is to prevent the mass from assuming a viscous condition. The slow cooling gives
time for the formation of crystals and as the crystals form, the remaining syrup
diffused through the mass becomes more dilute and fluid. After crystallisation,
the liquid is drained from the mass of crystals, preferably by means of a centrifugal
machine and thereby the larger portion of the liquid impurities are removed. The
resulting product will be found upon examination to be crystallized anhydrous
grape-sugar. This product may be washed with water or with a solution of pure
sugar, but even without washing will be found to be greatly improved in purity
and taste as compared with the original mass.
In this refining process it is necessary to exclude all traces of crystallized hydrate
of grape-sugar, otherwise a mixed crystallization will take place and the object of
the process be frustrated.
In refining grape-sugar by forming a crystallized hydrate it is necessary to arrest
the process of crystallization before completion, in order that there may remain in
the crystallized mass interstices sufficiently large to permit the expulsion of the
molasses or liquid impurities; but, owing to the nature of anhydride of grape-sugar,
especially the shape of its crystals, the process of crystallization may be allowed to
complete itself. The process of crystallization need not be arrested, because, as the
anhydride crystals are in the form of needles and prisms, their aggregation does
not prevent the existence of interstices large enough to permit the effectual
expulsion of the molasses or liquid impurities from the inass.
It will thus be seen that by my process of refining grape-sugar by forming the
crystallized anhydride, I am enabled to obtain a larger yield of crystals from a
given quantity of grape-sugar than can be obtained by forming therefrom the
crystallized hydrate.
The second part of my Invention is based upon the discovery of certain
conditions under which crystallized anhydride of grape-sugar may be produced
from a watery solution without the introduction into such solution of crystallized
anhydride previously prepared. These conditions are first, that the grape-sugar
shall be of great purity, so that the watery solution shall contain not less than
ninety-three parts of pure grape-sugar in one hundred parts of dry substance;
secondly, that the solution shall be concentrated until it contains not more than
fifteen per cent of water; and, thirdly, that after concentration the temperature
shall be reduced to a point at which proper crystallization will take place.
The required purification of the grape-sugar is most economically and effectually
accomplished by the method of refining which I have herein before described.
Ordinary grape-sugar may be less economically refined by forming crystallized
bydrate, but in such case, as 1 have already stated, it is necessary to arrest the
process of crystallization some time before it is completed, so that there may
remain in the crystallized mass interstices sufficiently large to permit the expulsion
of molasses or liquid impurities.
The next step in the second part of my Invention is to re-melt the crystals
obtained by the first step, and form therewith a solution containing not more than
fifteen per cent. of water. This solution or mass is then filled into moulds of
ordinary construction, and allowed to cool at a temperature of say 100° Fahrenheit
at about which temperature it is maintained for from twelve to twenty four bours.
During the latter part of the crystallizing operation, the temperature may, without
harm, be permitted to fall as low as 85° Fahrenheit. Under these circumstances
crystallization takes place. After crystallization is completed the mould is intro-
duced into a centrifugal machine, and, the liquid having been expelled and if

page_text: desired the sugar washed with a pure sugar solution, the crystallized mass is then
removed from the mould and dried at a low temperature. The product thus
obtained will, upon examination, be found to be crystallized anhydrous grape-sugar
of remarkable sweetness and purity.
The crystallized mass of anhydride is very hard, resembling block or loaf sugar
made from cane sugar, and it may be cut into lumps, or crushed or powdered.
It will be understood that any method of producing grape-sugar of upward of
ninety five per cent. in purity will answer the requirements of the second part of
my Invention. As ordinary grape-sugar is not sufficiently pure for my purpose I
have herein indicated an effectual method by which it may be relined.
It it be desired to produce a very pure hydrate of grape-sugar, the crystallized
anhydrous grape-sugar produced in the manner which I have described may be dis-
solved and again crystallized as hydrate, by introducing into the solution, while it
is at a moderate temperature, finely divided crystallized hydrate of grape-sugar and
treating the mass in the same manner as is now generally practiced for the
production of ordinary solid grape-sugar

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
4th July 1882.
WILLIAM ROBERT LAKE, of the Firm of Haseltine, Lake, & Co., Patent Agents,
Southampton Buildings, London, "IMPROVEMENTS IN AND RELATING TO THE
MANUFACTURE OF GRAPE-SUGAR"-A communication from abroad by Doctor
Arnot Behr, of Jersey City, New Jersey, United States of America, Chemist.
Crystallized grape-sugar, as heretofore produced from a watery solution, consists
of the hydrate of grape-sugar, containing in its pure state 9.09 per cent. of water
in chemical combination. This water is called "water of crystallization." The
crystallized hydrate of grape-sugar loses this water of crystallization if exposed to
a temperature of from 160° to 212° Fahrenheit. In form, the crystallized hydrate
is composed of spherical aggregations of minute tablets.
It has been known that crystallized anhydrous grape-sugar may be produced by
dissolving grape-sugar in strong alcohol and crystallizing it from this solution.
Anhydrous grape-sugar is distinguishable from the hydrate, first, by its crystalline
form, which is that of needles or prisms, and secondly, by the absence of water of
crystallization. When the anhydride is pure if it be expo-ed to a temperature of
from 160° to 212° Fahrenheit, it will not lose in weight, while, as has been
observed, the hydrate under similar circumstances, loses about nine per cent. of its
weight.
It is one object of the said Invention to produce crystallized anhydrous grape-
sugar, or in other words, crystallized anhydride of grape-sugar, from a watery
solution; and the first part of the said Invention is based upon the discovery of
certain conditions of concentration and temperature under which a watery solution
of ordinary commercial grape-sugar of fair purity-say eighty-five parts of pure
grape-sugar to one hundred parts of dry substance-can be made to deposit crys-
tallized anhydride of grape-sugar by mixing with it a small quantity of crystallized
anhydride of grape sugar, previously prepared.
The first part of the said Invention consists essentially in forming a watery
solution of ordinary commercial grape-sugar, containing not more than 15 per
cent of water; this solution is prepared at, or heated to, a temperature of from
140° to 180° Fahrenheit, and there is stirred into it a minute quantity, say one
hundredth per cent., of previously prepared finely divided anhydride of grape-
sugar. The hot mass is then deposited in moulds, in which it may be allowed to
rapidly cool down to about 100° Fahrenheit, from which point it is slowly cooled
to about 85° Fahrenheit, the time occupied in the slow cooling being from two to
three days, or until the contents of the moulds are thoroughly crystallized. The
object of the slow cooling is to prevent the mass from assuming a viscous condition.
The slow cooling gives time for the formation of crystals, and, as the crystals
form, the remaining sirup diffused through the mass becomes more dilute and fluid.
After crystallization, the liquid is drained from the mass of crystals, preferably by
means of a centrifugal machine, and thereby the larger portion of the liquid
impurities are removed. The resulting product will be found, upon examination,
to be crystallized anhydrous grape-sugar. This product may be washed with water,
or with a solution of pure sugar, but even without washing will be found to be
greatly improved in purity and taste as compared with the original mass.
In this refining process it is necessary to exclude all traces of crystallized
hydrate of grape-sugar, otherwise a mixed crystallization will take place, and the
object of the process will be frustrated.

page_text: In refining grape-sugar by forming a crystallized hydrate it is necessary to
arrest the process of crystallization before completion, in order that there may
remain in the crystallized mass interstices sufficiently large to permit the expulsion
of the molasses or liquid impurities; but, owing to the nature of anhydride of
grape-sugar, especially the shape of its crystals, the process of crystallization may
be allowed to complete itself. The process of crystallization need not be arrested,
because, as the anhydride crystals are in the form of needles and prisms, their
aggregation does not prevent the existence of interstices large enough to permit
the effectual expulsion of the molasses or liquid impurities from the mass.
It will thus be seen that by the said process of refining grape-sugar, by forming
the crystallized anhydride, I am enabled to obtain a larger yield of crystals from a
given quantity of grape-sugar than can be obtained by forming therefrom the
crystallized hydrate.
The second part of the said Invention is based upon the discovery of certain
conditions under which crystallized anhydride of grape-sugar may be produced
from a watery solution without the introduction into such solution, of crystallized
anhydride previously prepared. These conditions are, first, that the grape-sugar
shall be of great purity, so that the watery solution shall contain not less than
ninety-three parts of pure grape-sugar in one hundred parts of dry substance;
secondly, that the solution shall be concentrated until it contains not more than
fifteen per cent. of water; and thirdly, that, after concentration, the temperature
shall be reduced to a point at which proper crystallization will take place.
The required purification of the grape sugar is most economically and effectually
accomplished by the method of refining which I have hereinbefore described.
Ordinary grape-sugar may be less economically refined by forming crystallized
hydrate, but, in such case, as above stated, it is necessary to arrest the process of
crystallization some time before it is completed, so that there may remain in the
crystallized mass interstices sufficiently large to permit the expulsion of molasses or
liquid impurities.
The next step in the second part of the said Invention is to re-melt the crystals
obtained by the first step, and form there with a solution containing not more than
fifteen per cent. of water. This solution or mass is then filled into moulds of
ordinary construction, and allowed to cool to a temperature of say 100° Fahrenheit,
at about which temperature it is maintained for from twelve to twenty-four hours.
During the latter part of the crystallizing operation, the temperature inay without
harm be permitted to fall as low as 85° Fahrenheit. Under these circumstances
crystallization takes place. After crystallization is completed, the mould is
introduced into a centrifugal machine, and, the liquid having been expelled, and,
if desired, the sugar washed with a pure sugar-solution, the crystallized mass is
then removed from the mould and dried at a low temperature, The product thus
obtained will, upon examination, be found to be crystallized anhydrous grape-sugar
of remarkable sweetness and purity.
The crystallized mass of anhydride is very hard, resembling block or loaf-
sugar made from cane sugar, and it may be cut into lumps or crushed or powdered.
It will be understood that any method of producing grape-sugar of upward of
ninety five per cent. in purity, will answer the requirements of the second part of
the said Invention. As ordinary grape-sugar is not sufficiently pure for the
purpose of the said Invention, I have herein indicated an effectual method by which
it may be refined.
If it be desired to produce a very pure hydrate of grape-sugar, the crystallized
anhydrous grape-sugar, produced in the manner above described may be dissolved
and again crystallized as hydrate, by introducing into the solution, while it is at a
moderate temperature, finely-divided crystallized hydrate of grape-sugar, and
treating the mass in the same manner as is now generally practised for the
production of ordinary solid grape sugar.
Having thus fully described the said Invention as communicated to me by my

page_text: foreign correspondent and the manner of performing the same I wish it under-
stood that I do not claim broadly the employment of previously prepared
crystallized sugar for facilitating the crystallization of a sugar solution, as the first
part of my Invention is limited to the use of crystallized anhydride of grape-
sugar in a watery solution of grape-sugar under the conditions of concentration
and temperature which I have described, but I claim :-
First. The method of refining grape-sugar herein described, which consists in
forming a hot solution of ordinary commercial grape-sugar containing not more
than fifteen per cent. of water, stirring into such solution a minute quantity of
finely divided crystallized anhydride of grape-sugar previously prepared, and then
depositing the hot mass in moulds and allowing it to rapidly cool to about 100°
Fahrenheit, and thereafter cooling it slowly, maintaining it at a temperature of
between 100° and 85° Fahrenheit for from two to three days, or until thorough
crystallization has taken place, after which the resulting hard mass of crystals is
drained, preferably in a centrifugal machine, and thereby the molasses or liquid
impurities are expelled, all substantially as set forth and for the purposes specified.
Second. The process of manufacturing crystallized anhydride of grape-sugar
herein described, which consists in forming a solution, containing not more than
fifteen per cent. of water, with grape-sugar of upward of ninety-five per cent. in
purity, filling such solution or mass into moulds of ordinary construction, and
cooling it to a temperature preferably of about 100° Fahrenheit, and maintaining
it at about that temperature for from twelve to twenty-four hours, or until
thorough crystallization has taken place, and then expelling the liquid therefrom
by means of a centrifugal machine, all substantially as set forth and for the
purposes specified.
In witness whereof I the said William Robert Lake have hereunto set my
hand and seal this Fourth day of July in the year of our Lord Oue
thousand eight hundred and eighty two.
W. ROB. LAKE.
(L.S.)