IMPROVEMENTS IN THE PREPARATION OF ANIMAL 41E1
Year: 1870

page_text: LETTERS PATENT to William Thurston, Waite, of the Town and
County of Southampton, Fellow of the Chemical Society of London,
for the Invention of "IMPROVEMENTS IN THE PREPARATION OF ANIMAL
41E1
PROVISIONAL SPECIFICATION left by the said William Thurston Waite
at the Office of the Commissioners of Patents, with his Petition, on'
the 22nd January 1870.
"
I, WILLIAM THURSTON WAITE, of the Town and County of South-
ampton, Fellow of the Chemical Society of London, do hereby declare.
the nature of the said' Invention for “IMPROVEMENTS IN THE PREPARATION.
OF ANIMAL CHARCOAL FOR USE IN TREATING SACCHARINE SOLUTIONS," to be as
follows:
My Invention relates to the treatment of animal charcoal in order to
render it more effective in the purification or treatment of saccharine
solutions.
.....
On the 8th January 1869 Letters Patent (No. 62) were granted
to me for the use of certain substances for purifying saccharine

page_text: solutions, one of such substances being a mixture of phosphate of lime
which had been prepared by precipitation and carbon. In the Specifi-
cation of the said Letters Patent I stated that this mixture might be
obtained by mixing together powdered animal charcoal, sulphuric acid,
and water in certain proportions, allowing them to stand for a time and
then adding lime, stirring the whole well together, the result being that
the phosphate of lime in the charcoal was formed into an insoluble finely
divided precipitate. When the mixture of phosphate of lime and carbon
is made in the manner just described it has mixed with it a large pro-
portion of sulphate of lime, which is practically a great inconvenience,
and if hydrochloric acid or any other acid which forms soluble salts with
lime be substituted, as these soluble salts of lime are injurious to the
saccharine solutions, they have to be completely removed from the
mixture of phosphate of lime and carbon by long continued washings,
and this is also inconvenient and difficult to manage. Again if I sub-
stitute phosphoric acid simply I get neither sulphate of lime nor soluble
salts of lime, but I obtain such a greatly increased proportion of
phosphate in the mixture obtained that it is not nearly so efficient for
the purpose as if it contained a less proportion.
For the purpose then of obtaining a comparatively pure mixture of
carbon and precipitated phosphate of lime in advantageous proportions
I proceed as follows:-I take, say, 100 parts of animal charcoal, and put
therewith an aqueous solution of phosphoric acid consisting of about
2000 parts of water. holding in solution about 200 parts of phosphoric
acid. By preference I first prepare the acid solution and note its volume
and then put the animal charcoal into it; I mix them thoroughly and
let the mixture stand for some time, say from 6 to 12 hours, when nearly
the whole of that portion of the animal charcoal which has not been
dissolved will have subsided to the bottom of the vessel in which the
mixture is contained; I then decant, draw off, or otherwise.remove from
it a quantity of the liquor equal in volume to about five-sixths of the
volume of the original solution of phosphoric acid, this liquor should.be
drawn off as free from insoluble matter as practicable; I then add about
500 parts of water to the sixth, which remains mixed with the insoluble
matter and stir them well together, after which I pour the mixture into
a cream of lime prepared by slaking about 32 parts of lime and mingling
I stir well while the
with it from 500 to 1000 parts of water.
phosphate is running into the cream of lime, and I thoroughly mix them

page_text: together and allow the mixture to stand for some time, say from 6 to
12 hours, stirring it occasionally. It may then be allowed to subside and
as much of the water as convenient may be run away from it, when it is
ready to be put into the saccharine solution, or it may be first partially
dried. By this means I form a comparatively pure mixture of carbon
and precipitated phosphate of lime in proportions advantageous for the
purpose of purifying saccharine solutions.
.
To prepare a solution of phosphoric acid for the next operation I take
the five-sixths of the liquor drawn off as previously stated and add to
it about 70 parts of sulphuric acid, this will form a sulphate with the
lime in the solution which will be precipitated; the clear liquor, which is
a solution of phosphoric acid, is then drawn off and the last portions of
it removed from the precipitated sulphate of lime by washing.
Another mode or process of preparing a mixture of carbon and
precipitated phosphate of lime is as follows:-I take, say, 100 parts of
animal charcoal and mix. therewith about 500 parts of water; I then
pass sulphurous acid gas into the mixture until the gas ceases to be
absorbed and allow the mixture to stand for, say, from 6 to 12 hours; I
then remove the solution as completely as practicable from the undis-
solved portions, place it in a suitable vessel, and add to it about 50 parts
of sulphuric acid. The greater portion of the lime is thus converted
into sulphate of lime and the sulphurous acid is liberated. I then boil
the solution to drive off as much as possible of the sulphurous acid,
which may be used again as before; the solution is next separated from
the sulphate of lime and mixed with the undissolved portions of the
animal charcoal, they are stirred together and poured into a cream of
lime as described for the former process, using in this case about
26%, parts of lime.
N
I do not limit myself to the use of sulphurous acid as other sufficiently
volatile acids might answer the purpose, nor do I limit myself to the
proportions herein-before given as they will vary according to circum-
stances.
Although in the methods described the phosphatic solution and the
insoluble matter of the animal charcoal are mixed together when the
lime is added for the purpose of forming my precipitate, yet if necessary
the phosphatic solution could be obtained separately and the lime added
to it, and the other insoluble portion of the charcoal added to it after
the precipitate is formed..

page_text: 1
If it be thought desirable to have a less proportion of phosphate of
lime in the mixture and obtain a by-product of phosphoric acid or a
phosphate, this result may be attained in the first process herein-before
described by withdrawing a portion of the solution remaining after five-
sixths have been taken away as explained; the portion thus withdrawn
contains the by-product, but of course in this case a less proportion of
lime must be employed to precipitate the remainder. A like result may
be obtained, in the second process; by adding only a portion of the liquor
which has been withdrawn from the sulphate to the insoluble portions of
the animal black, the portion of the liquor which remains forming the
by-product.
SPECIFICATION, in pursuance of the conditions of the Letters Patent,
filed by the said William Thurston Waite in the. Great Seal Patent
Office on the 22nd July 1870.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, WILLIAM
THURSTON WAITE, of the Town and County of Southampton, Fellow of
the Chemical Society of London, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Twenty-second day of January, in the
year of our Lord One thousand eight hundred and seventy, in the
thirty-third year of Her reign, did, for Herself, Her heirs and successors,
give and grant unto me, the said William Thurston Waite, Her special
licence that I, the said William Thurston Waite, my executors, adminis-
trators, and assigns, or such others as I, the said William Thurston
Waite, my executors, administrators, and assigns, should at any time
agree with, and no others, from time to time and at all times there-
after 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 THE PREPARATION OF ANIMAL CHARCOAL FOR USE IN
TREATING SACCHARINE MATTERS," upon the condition (amongst otliers) that
I, the said William Thurston Waite, 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,

page_text: 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 William Thurston Waite, do hereby
declare the nature of my 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:
My Invention relates to the treatment of animal charcoal in order to
render it more effective in the purification or treatment of saccharine
solutions.
:
On the 8th January 1869 Letters Patent (No. 62) were granted
to me for the use of certain substances for purifying saccharine
solutions, one of such substances being a mixture of phosphate of lime
which had been prepared by precipitation and carbon. In the Specifica-
tion of the said Letters Patent I stated that this mixture might be
obtained by mixing together powdered animal charcoal, sulphuric acid;
and water in certain proportions, allowing them to stand for a time,
and then adding lime, stirring the whole well together, the result being
that the phosphate of lime in the charcoal was formed into an insoluble
finely divided precipitate.
F
When the mixture of phosphate of lime and carbon is made in the
manner just described it has mixed with it a large proportion of
sulphate of lime, which is practically a great inconvenience, and if hydro-
chloric acid or any other acid which forms soluble salts with lime be
substituted, as these soluble salts of lime are injurious to the saccharine
solutions they have to be completely removed from 'the 'mixture of
phosphate of lime and carbon by long continued washings, and this is
also inconvenient and difficult to manage. Again, if I substitute
phosphoric acid simply I get neither sulphate of lime nor soluble salts.
of lime, but I have such a greatly increased proportion of phosphate in
the mixture obtained that it is not nearly so efficient as if it contained
a less proportion.
:
For the purpose then of obtaining a comparatively pure. mixture of
carbon and precipitated phosphate of lime in advantageous proportions
I proceed as follows:-I take, say, 100, parts of animal charcoal and put
therewith an aqueous, solution of phosphoric acid consisting of about
3000 parts of water holding in solution about 80 parts of phosphoric

page_text: '
acid.. By preference I first prepare the acid solution and note its
volume, and then. put. the animal charcoal: into it. I mix them
thoroughly and let the mixture stand for some time, say from 6 to 12
hours, when nearly the whole of that portion of the animal, charcoal
which has not been dissolved will have subsided to the bottom of the
vessel in which the mixture is contained; I then decant, draw off, or
otherwise remove from it a quantity of the liquor equal in volume to
about two-thirds of the volume of the original solution of phosphoric
acid; this liquor should be drawn off as free from insoluble matter-as
practicable; I then add about 500 parts of water to the third which
remains mixed with the insoluble matter and stir them well together,
after which I pour the mixture into a cream of lime prepared by slaking
about 28 parts of lime and mingling with it from 500 to 1000 parts of
water. I stir well while the phosphate is running into the cream of
lime, and I thoroughly mix them together and allow the mixture to
stand for some time, say from 6 to 12 hours, stirring it occasionally.
It may then be allowed to subside, and as much of the water as con-
venient may be run away from it, when it is ready to be put with
the saccharine solution, or it may be first partially dried.
By this
means I form a comparatively pure mixture of carbon and precipitated
phosphate of lime in proportions advantageous for the purpose of
purifying saccharine solutions.
To prepare a solution of phosphoric acid for the next operation I take
the two-thirds of the liquor drawn off as previously stated and add to it
about 60 parts of sulphuric acid; this will form a sulphate with the lime
in the solution which will be precipitated; the clear liquor, which is a
solution of phosphoric acid, is then drawn off and the last portions of it
removed from the precipitated sulphate of lime by washing.
I have found in practice that a good result may also be obtained by
using a larger proportion of phosphoric acid having a proportion of lime
already dissolved in it.
The process as thus modified' will be as follows:-I take an aqueous
solution of phosphoric acid and lime consisting of about 6000 parts of
water holding in solution about 160 parts of phosphoric acid and about
30 parts of lime. I note its volume and then put with it about 100 parts a
of animal charcoal. I stir them thoroughly well together and allow
them to stand for from 1 to 6 hours, and I then draw off about four-
fifths of the liquor;: I then add about 500 parts of water to the fifth

page_text: which remains mixed with the insoluble matter and stir them well
together, after which I pour the mixture into a cream of lime prepared
by slaking about 28 parts of lime and mingling with it from 500 to 1000
parts of water; I then continue the rest of the process exactly in the
manner herein-before stated.
1
Si
To prepare a solution of phosphoric acid and lime for the next
operation I take the four-fifths of the liquor drawn off, as previously
stated and add to it about 60 parts of sulphuric acid, and then proceed
as in the former process, but the solution which I have spoken of as
phosphoric acid and lime will in this case perhaps be more strictly
speaking considered a solution of phosphate of lime containing a large
amount of phosphoric acid in proportion to the lime.
:
. [
*
.
Another mode or process of preparing a mixture of carbon and
precipitated phosphate of lime is as follows:-I take, say, 100 parts of
animal charcoal and mix therewith about 500 parts of water; I then
pass sulphurous acid gas into the mixture until the gas ceases to be
absorbed, and allow the mixture to stand, say, from 6 to 12 hours; I
then remove the solution as completely as practicable from the undis-
solved portions, place it in a suitable vessel, and add to it about 50 parts
of sulphuric acid. The greater portion of the lime is thus converted into
sulphate of lime and the sulphurous acid is liberated; I then boil the
solution to drive off as much as possible of the sulphurous acid, which
may be used again as before. The solution is next separated from the
sulphate of lime and mixed with the undissolved portions of the
animal charcoal; they are stirred together and poured into a cream of
lime as described for the first process, using in this case about 26½ parts
of lime.
I do not limit myself to the use of sulphurous acid as other sufficiently
volatile acids would answer the purpose, nor do I limit myself to the
proportions herein-before given, as they will vary according to
circumstances.
Although in the method described the phosphatic solution and the
insoluble matter of the animal charcoal are mixed together when the

page_text: If it be thought desirable to have a less proportion of phosphate
of lime in the mixture and obtain a by-product of phosphoric acid
or a phosphate this result may be attained in the first process herein-
before described by withdrawing a portion of the solution remaining
after two-thirds have been taken away as explained; the portion
thus withdrawn contains the by-product, but of course in this case
a less proportion of lime must be employed to precipitate the re-
mainder. A like result may be obtained in the last process by adding
only a portion of the liquor which has been withdrawn from the sulphate
to the insoluble portions of the animal black, the portion of the liquor 1
which remains forming the by-product.
In witness whereof, I, the said William Thurston Waite, have
hereunto set my hand and seal, this Nineteenth day of July One
thousand eight hundred and seventy.
WILLIAM THURSTON WAITE. (L.S.)