IMPROVEMENTS IN PREPARING CHARCOAL FOR DECOLORISING SYRUPS AND OTHER SOLUTIONS
Year: 1870

page_text: LETTERS PATENT to George Phillips, of No. 74, Tufnell Park Road,
in the County of Middlesex, Analytical Chemist, for the Invention
of "IMPROVEMENTS IN PREPARING CHARCOAL FOR DECOLORISING SYRUPS AND
OTHER SOLUTIONS."
Sealed the 24th September 1870, and dated the 20th July 1870.
PROVISIONAL SPECIFICATION left by the said George Phillips at the
Office of the Commissioners of Patents, with his Petition, on the
20th July 1870.
I, GEORGE PHILLIPS, of No. 74, Tufnell Park Road, in the County of
Middlesex, Analytical Chemist, do hereby declare the nature of the said
Invention for "IMPROVEMENTS IN PREPARING CHARCOAL FOR DECOLORISING
SYRUPS AND OTHER SOLUTIONS," to be as follows:-
I take animal or other suitable charcoal and grind it in water until
reduced to an impalpable state, that which is suspended in the water I
pour off and collect either by subsidence or filtration and treat in the
following manner :-I take ethylic, common, vinous alcohol, or methylic

page_text: alcohol, known as wood spirit, or a mixture of these two, known as
methylated spirit, and I add to the alcohol to be employed either
caustic ammonia, known as liquor ammonia, or caustic soda, potash,
or lithia, or any of their salts having causticity and that are soluble in
the alcohols named. To the alcohol thus rendered caustic I add the
impalpable charcoal and heat up in the case of the ammonia alcohol
to from 100° to 130° Fahrenheit. In the case of alcohol and the three
fixed alkalies named I heat to 180° Fahrenheit, using proper means such
as cohobation and sufficient condensing power to prevent loss of material.
I continue the heat for about one hour or more, according to circum-
stances, the caustic alcohol is then run off into a properly arranged
distilling apparatus, redistilled, and collected for future use. The animal
and other similar charcoal thus prepared is much improved in decolorizing
power, and in the case of animal charcoal used in decolorizing saccharine
solutions such as bane, beet, glucose, or fruit sugars, the power is greatly
increased.
Of the alkalies named I prefer ammonia on account of the easy manner
in which the charcoal can be freed from it. I take ethylic alcohol in
preference and of a strength varying in density from 8805 to 920 at 60°
Fahrenheit, and to this I add one-twentieth of its bulk of liquor ammonia'
of from 8.00 to 8.70 density at 60° Fahrenheit and heat in the way
described. If the animal charcoal be new charcoal that has never been
used a large quantity of colouring matter as well as the offensive smell
will be taken from it; if it be animal charcoal that has been used in
decolorizing saccharine solutions the coloring matter taken from the
sugars will be dissolved out, and the charcoal when dried by any suitable
steam or other arrangement will be fit for use without being removed
from the vessel in which it has been placed to decolorize the saccharine
solution. If the fixed alkalies named be used, the charcoal must be washed
until freed from their presence, and the quantity of the fixed alkalies
to be added to the alcohol employed should be such that the alcohol
has a strong alkaline reaction.
.
In preparing new charcoal or after it has been used I do not
confine myself to the impalpable form, though I prefer it as charcoal
as ordinarily used in decolorizing sugar solution can be treated in
the manner I have described and rendered more powerful in its
action. In the case of saccharine solutions the coloring matter taken
up by the charcoal is insoluble in water and in alcohol varying in

page_text: density at 60° Fahrenheit from 8376 to absolute alcohol. Alcohol
.without admixture of alkali may be used for the treatment of charcoal
as above described, but the use of alkali renders it more effective.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said George Phillips in the Great Seal Patent Office
on the 19th January 1871.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, GEORGE
PHILLIPS, of No. 74, Tuffnell Park Road, in the County of Middlesex,
Analytical Chemist, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Twentieth day of July, in the year of
our Lord One thousand eight hundred and seventy, in the thirty-fourth
year of Her reign, did, for Herself, Her heirs and successors, give and
grant unto me, the said George Phillips, Her special license that I,
the said George Phillips, my executors, administrators, and assigns,
or such others as I, the said George Phillips, my executors, adminis-
trators, and assigns, should at any time agree with, and no others,
from time to time and at all times thereafter during the term therein
expressed, should and lawfully might make, use, exercise, and vend,
within the United Kingdom of Great Britain and Ireland, the Channel
Islands, and Isle of Man, an Invention for "IMPROVEMENTS IN PREPARING
CHARCOAL FOR DECOLORISING SYRUPS. AND OTHER SOLUTIONS," upon the con-
dition (amongst others) that I, the said George Phillips, my executors
or administrators, by an instrument in writing under my, or their, or
one of their hands and seals, should particularly describe and ascertain
the nature of the said Invention, and in what manner the same was
to be performed, and cause the same to be filed in the Great Seal
Patent Office within six calendar months next and immediately after
the date of the said Letters Patent.
NOW KNOW YE, that I, the said George Phillips, do hereby declare
the nature of the said Invention, and in what manner the same is to
be performed, to be particularly described and ascertained in and by the
following statement thereof, that is to say :-
This Invention has for its object improvements in preparing charcoal
for decolorizing syrups and other solutions.

page_text: I take animal or other suitable charcoal having sufficiently marked
decolorizing properties, and grind it.in water until reduced to an impal-
pable state; that which is suspended in the water I pour off and collect,
either by subsidence or filtration, and treat in the following manner :—
I take ethylic (common vinous) alcohol or methylic alcohol, known as
wood spirit, or a mixture of these two, known as methylated spirit, and
I add to the alcohol to be employed either caustic ammonia or caustic
soda, potash, or lithia, or any of their salts having causticity, and that
are soluble in the alcohols named. To the alcohol thus rendered
caustic I add the impalpable charcoal, and heat up in the case of the
ammonia alcohol to from 100° to 130° Fahrenheit. In the case of
alcohol and the three fixed alkalies named I heat to 180° Fahrenheit,
using proper means, such as cohobation and sufficient condensing power,
to prevent loss of material. I continue the heat for about one hour or
more according to circumstances; the caustic alcohol is then run off
into a properly arranged distilling apparatus, redistilled, and collected
for future use.
The animal and other similar charcoal thus prepared
is much improved in decolorising power.
Of the alkalies named I prefer ammonia on account of the easy
manner in which the charcoal can be freed from it. I take ethylic 2
alcohol in preference, and of a strength varying in density from '8805
to 920 at 60° Fahrenheit, and to this I add one-twentieth of its bulk
of liquor ammonia of from 800 to 870 density at 60° Fahrenheit, and
heat in the way described. If the animal charcoal be new charcoal
that has never been used, a large quantity of coloring matter in some 2
cases as well as the offensive smell, will be taken from it; if it be animal
charcoal that has been used in decolorising saccharine solutions the
coloring matter taken from the sugar will be dissolved. out, and the
charcoal when dried by any suitable steam or other arrangement will be
fit for use without removal from the vessel in which it has been placed 3
to decolorise the saccharine solution. If the fixed alkalies named be
used the charcoal must be washed until freed from their presence, and
the quantities of the fixed alkalies to be added to the alcohol employed
should be such that the alcohol has a strong alkaline reaction.
I do not confine myself to the impalpable form of the charcoal, 3
though I prefer it, as charcoal as ordinarily used in decolorising sugar
solution can be treated in the manner I have described and rendered
more powerful in its action.

page_text: be used, but as the use of the alkalies renders it more effective I prefer
their admixture.
The way in which I prefer to use charcoal in decolorising solutions
of sugar and other solutions containing color capable of being removed
by charcoal and dissolved by the solvents herein named is as follows:-
I take by preference animal charcoal prepared in the way described and
place it in a suitable vessel containing an axis with stirring arms. This
vessel is so arranged that it can be closed at the top and bottom, with
_ proper outlets at command, so as to form a still, and with a false bottom
consisting of two perforated metal plates with flannel or other close fabric
between them so as to form a filter. The decolorisation having been effected
in the manner herein-after set forth, and the liquid run off from the char-
coal and the charcoal washed, the next stage may be proceeded with,
videlicet, the freeing of the charcoal of the coloring matter it has taken
up in the way herein described. Alcohol is poured upon the charcoal,
and as the moist charcoal contains from forty to fifty per cent. of water,
the alcohol should be added in such strength and quantity that when
combined with the water of the charcoal its density shall be within the
range of the densities from 8805 to 920. If (as I prefer) ammonia be
employed together with alcohol I take four parts of alcohol and add
one part of liquor ammonia of a density of from 800 to 880 at 60°
Fahrenheit, and apply the mixture to the charcoal in the vat as already
described. I next by means of a coil of steam pipes in the vat or by
other means heat it up to from 100° to 130° Fahrenheit, with proper.
means to prevent loss of material if any exit exists from the vessel. I
continue the heat for one hour or more, then filter away, and run off
the liquid into a properly arranged distilling apparatus, and recover the
liquid free of coloring matter for future use. The charcoal in the vat
is now by means of the steam pipes or by free steam blown into the
vat, or otherwise heated or raised to a temperature of 180° Fahrenheit, and
the remaining alcohol and ammonia, as the case may be, is distilled over
and recovered in the usual manner. In cases where the charcoal is
much loaded with coloring matter it may be found advisable to repeat
the ammonia alcohol treatment. The charcoal being thus prepared the
syrup or solution of sugar or other solution is again run upon it, and
the whole well stirred up for about five minutes, and the syrup or solution

page_text: is filtered off. The filtration may be accelerated by air pressure or by
exhaust. The charcoal is next washed to remove the remaining sugar or
matter, it is then again submitted to the alkaline alcoholic treatment,
and so the same charcoal is used over and over again an indefinite number
of times. In a properly arranged vessel there should-be little or no loss
of alcohol and ammonia. Before repeating the alkaline alcoholic treat-
ment the charcoal may with advantage be boiled with water. If fixed
alkalies are used I simply make the alcohols moderately alkaline, and
heat up to from 170° to 180 Fahrenheit. The same treatment as to
the recovery of the alcohol may be pursued, and after this the charcoal
must be washed with water until the water passes free from alkalinity.
As the different kinds of sugar contain variable amounts of coloring
matter the quantity of charcoal necessary in each case will be dependent
on the amount of coloring matter to be removed, but in all cases
I find it advantageous to use an excess, and to decolorize in about five
minutes. The quantity of the charcoal to effect this may be readily
ascertained by treating one hundred grains of the sugar with one
thousand grains of common or pure water and adding if it be good
raw sugar one hundred grains of the prepared charcoal, and well
agitating the whole in a glass stoppered bottle for five minutes. If
upon filtering the liquid it be quite colorless, and if when the charcoal
is well washed with water the washing is also colorless, the quantity of
charcoal employed is sufficient, if not colorless all through the solutions.
and washings more charcoal is required. In the lowest descriptions
of sugar used for refining purposes I have found six times the weight
of the prepared charcoal always perfectly decolorises it in five minutes.
As the charcoal by my process is improved in power by use the quantity
is not a consideration, as no loss occurs, and as I hold that to some
extent the quantity of pure sugar produced is dependent on the time
employed in decolorising I recommend that it be effected in the shortest
possible time. I prefer the sugar solutions to be made without heat
being employed, and decolorised while cold, and as regards the quantity
of water to be employed I prefer much thinner solutions than those
now used.
It is the practice pretty generally now in refining to use a
solution of about 28° Beaumé, or equal weights of sugar and water, and
this hot. I recommend cold solutions and from four to ten parts of
water to one part of sugar by weight, and brisk agitation of the sugar
solution with the charcoal for five minutes. The objection that appears
to this is the increased amount of water to be evaporated, but this is

page_text: compensated for by the rapidity and perfection of the process. However,
the present mode of solution and scale of dilution can be maintained
where desired.
What has been stated relates to all substances with which prepared
charcoal can be used as a decoloriser, and the solvents herein named are
solvents of the coloring matter thus taken up by the charcoal.
Having thus described the nature of my said Invention, and the
manner of performing the same, I would have it understood that I
claim the preparation of animal or other charcoal for decolorising syrups
and other solutions by treating it with ethylic alcohol or other alcohol,
substantially as described.
I also claim the preparation of animal and other charcoal for deco-
lorising syrups and other solutions by treating it with ethylic alcohol
or other alcohol, together with ammonia and other alkali or alkaline
substance, substantially as described.
In witness whereof, I, the said George Phillips, have hereunto set
my hand and seal, this Sixteenth day of January, in the year
of our Lord One thousand eight hundred and seventy-one.