CERTAIN IMPROVEMENTS IN MANUFACTURING, COLOURING MATTER, AND RENDERING CERTAIN COLOUR. OR COLOURS. MORE. APPLICABLE TO DYEING, STAINING, AND WRITING
Year: 1837

page_text: TO ALL TO WHOM THESE PRESENTS SHALL COME, I, HENRY
STEPHENS, of Charlotte Street. in the Parish of Saint Marylebone; in the
County of Middlesex, Gentleman, send greeting.
WHEREAS His late most Excellent Majesty King William the Fourth,
by His Royal Letters Patent under the Great Seal of Great Britain, bearing
date at Westminster, the Eighteenth day of April, in the seventh year of His
reign, and in the year of our Lord One thousand, eight. hundred and thirty-
seven, did, for Himself, His heirs and successors, give and grant unto me, the
said Henry Stephens, and EBENEZER NASH, of Bross Street, in the Parish of
Saint George in the East, and County of Middlesex, Tallow Chandler, His
especial license, full power, sole privilege and authority, that we, the said
Henry Stephens and Ebenezer Nash, our executors, administrators, and
assigns, or such others as we, the said Henry Stephens, and Ebenezer Nash,
our executors, administrators, or assigns, should at any time agree with,
and no others, from time to time and at all times during the term of years
therein mentioned, should and lawfully might make, use, exercise, and
vend, within England, Wales, and the Town of Berwick-upon-Tweed, our
Invention of "CERTAIN IMPROVEMENTS IN MANUFACTURING, COLOURING MATTER,
AND RENDERING CERTAIN COLOUR. OR COLOURS. MORE. APPLICABLE TO DYEING,
STAINING, AND WRITING;" in which said Letters Patent is contained a pro-
viso obliging us, the said. Henry Stephens. and. Ebenezer Nash, by an
instrument in writing under our hands and seals, or under the hand and
seal of one of us, particularly to describe and ascertain the nature of out
1

page_text: said Invention, and in what manner the same is to be performed, and
to cause the same to be inrolled in His Majesty's High Court of Chancery
within six calendar months next and immediately after the date of the said
in part recited Letters Patent, as in and by the same, reference being
thereunto had, will more fully and at large appear.
NOW KNOW YE, that in compliance with the said proviso, I, the said
Henry Stephens (on behalf of myself and of the said Ebenezer Nash) do
hereby declare that the nature of our said Invention, and the manner in
which the same is to be performed, are particularly described and ascertained
in and by the following description thereof, reference being had to the Drawings
hereunto annexed, and to the letters and figures marked thereon (that is
to say):
Our improvements in manufacturing colouring matter and rendering
certain colour or colours more applicable to dyeing, staining, and writing,
consist, in the first place, of several improvements in making or manufacturing
the ferro-prussiates (that is, prussiates of potash and soda); secondly, in
rendering Prussian blue soluble, and thereby more applicable than heretofore
to the purposes of dyeing, staining, colouring, or writing; thirdly, in a peculiar
manner or method of treating or operating upon cochineal and on lac dye by
combining the coloring matter of cochineal or of lac dye with other matters so
as to produce a superior red fluid applicable to writing, staining, or colouring;
and, fourthly, in combining carbon with the above-described solution of
Prussian blue or any other colours so as to form a writing fluid or ink which
cannot be entirely effaced by chemical agents: all of which improvements we
are now about to describe under different heads or sections (that is to say):-
Our first improvement consists in converting certain gaseous products
arising from the present mode of making prussiate of potash or soda from
animal matter (which are now commonly allowed to escape into the atmosphere)
to the purpose of making prussiate of potash or soda, so that an increased
quantity of prussiate of potash or soda may be obtained from a given quantity
of animal matter. For the better explanation of this part of our Invention
we refer to the annexed Drawings, in which Figure 1 represents an apparatus
for effecting the process of converting the gas evolved into prussiate. a is an
iron pot, vessel, or retort, charged with alkali and animal or other matter
containing azote or yielding ammonia, which vessel is to be heated to a low
red heat. This pot or vessel has a moveable cover, which is to be luted on
when under operation, but may be removed and placed upon another pot b by
disconnecting the joint in the pipe c, the joint allowing the head of the pot a
to be carried round with the connecting pipe c. The pipe c is for conducting

page_text: the gaseous products arising from the decomposition of the said animal matter
in the pots a or b into an iron cylindrical or other conveniently-shaped vessel d,
heated by a furnace below. This vessel d is to be charged with alkali, and
to be kept at a full red heat during the operation. e is a pipe leading from
the cylindrical vessel io a closed vessel containing a solution of alkali. This
vessel is furnished with a jet pipe or burner g. which is merely intended as a
gauge cock to ascertain the state of the gas. i, i, are furnaces under the
parts a and b. The gas generated in the retort a passes, by the connecting
pipe c, to the cylinder d, where, meeting with the alkali in a state of fusion,
the effect will be that the gas becomes combined to a certain degree with the
alkali and forms prussiate of potash or soda. But there may be portions of
the said gas which do not combine or commix with the alkali; these will
pass off by the pipe e to the closed vessel f, and if any of the gas thus
passed off should be capable of combining with the alkaline solution it
may do so in the closed vessel, and that portion which does not com
bine with the alkaline solution is allowed to pass off by the gas-jet pipe g:
The state of operation may be ascertained by burning the jet gas from
the end of this pipe: for when it ceases to burn freely the connection
between the pot a and cylinder d should be disconnected, and the head
and pipe c be removed round and luted on to the pot b. which is to be
previously charged with animal matter and alkali, the distillation of which
will proceed as before described. When the gaseous products of several
charges have been passed through the cylinder d containing the alkali the
cylinder may be opened, and the charge (which will now consist of crude
prussiate of potash or soda, or "metal" as it is commonly called in the trade)
be withdrawn into an iron vessel, and when cold be lixiviated in cold water in
the usual manner. The further decomposition of the charge of animal matter
in the pot a may now he conducted in the ordinary manner of making
prussiate in the open vessel by increasing the heat, the contents being
agitated as usual. This process may be repeated alternately in the two pots
a and the completion of the decomposition of the charge of one being
effected while that of the other is subjected to the lower heat, and the operation
of distilling off its vapours and passing it to the retort or vessel c. A similar
effect. (viz) that of taking up the gaseous products so as to produce an
additional quantity of crude prussiate of potash or "metal" may be obtained.
by placing in an open conical chimney, having à false bottom or grating or
perforated plate, upon which dry potash or soda is placed, so that the gas
generated in the pot below may pass through the stratum of alkali in the
chimney.

page_text: Fig. 2 is a sectional elevation representing this application of the improve-
ment. E is the chimney or open cone usually placed on the top of an
ordinary pot F for making prussiate of potash, in order to convey the flame
upwards. G is a grating or perforated plate placed at the base of the cone E.
Upon this grating or perforated plate G a stratum of dry potash or soda is
laid, and as the gas passes upward through this stratum a portion of it
will become combined with the alkali. The chimney, with the stratum
of alkali, may be removed when the flame begins to burn weak, and it may be
set aside and applied to future charges, or put into the pot and worked off
with the charge in the usual manner of making prussiate of potash or soda.
Our second improvement-(viz) the mode, method, or process of treating or
operating upon Prussian blue, so as to render it more perfectly soluble, or more
readily disposed to be acted upon by the subsequent process of solution than
when manufactured in the usual way, and in order that the same may be more
applicable to the purposes of dyeing, staining. colouring, and writing-we effect.
in the following manner:We take the Prussian blue, whether produced from
a combination of prussiate of potash and salts of iron, or the Prussian blue of
commerce, as commonly manufactured, and we put this into an earthen vessel,
and pour over it a quantity of strongly concentrated acid, sufficient to cover
the Prussian blue; muriatic acid, sulphuric acid, or any other acid which has a
sufficient action upon iron will do. If sulphuric acid is used it should be
diluted a little, that is, with a quantity of water equal to about its bulk, at the
time when the mass turns white after the Prussian blue is put in. The
Prussian blue is to be allowed to remain in the acid from twenty-four to
forty-eight hours or longer. We then dilute this mixture with a large quantity
of water, stirring it up at the time for the purpose of washing from it the salis
of iron. When in this state of dilution we suffer it to stand until the colour
has subsided, when the supernatant liquor is to be drawn off with a syphon,
and more water added to it. and we continue the repetition of this process
until we judge that the acid with the iron has been completely washed away.
and this is known by testing it with prussiate of potash. which will shew if i
yields any blue precipitate. if not it is sufliciently washed: we then place it
mpon a filter and suffer it to remain until the liquid has all drained away. The
Prussian blue thus prepared is reduced to a state as we conceive containing less
iron than the Prussian blue of commerce, in which state it is more readily
acted upon and rendered soluble than in any other condition. This Prussian
blue may be then placed in evaporating dishes, and gently dried. To form the
Prussian blue so operated upon into a solution we add to it oxalic acid, and
mix them carefully together. after which we add coal water (cold distilled

page_text: water is best) a little at a time, making it into a dense or dilute solution.
according to the colour required. The quantity of oxalic acid may vary
according to the quantity of water used. It will be found that the Prussian
blue that has undergone the process of digestion, as described. requires but a
small quantity of oxalic acid to dissolve it. About one part of oxalic acid will
dissolve six parts of Prussian blue (the weight taken before digesting in the
acid). This will answer for a concentrated solution, but for a dilute solution
more acid will be required. Prussian blue that has not undergone digestion
in acid in the way above pointed out will require a much larger proportion
of oxalic acid from twice to three times its weight, and even then it will be
greatly liable to precipitation after standing. but when treated in the way
described it is not liable to precipitate, but remains a permanent solution. The
chief obstacle to the general employment of the beautiful colour obtained by
means of the ferro-prussiates to the purposes of dyeing in the silk, cotton. linen,
or woollen manufactures, and also to the purposes of staining and writing, has
been its hitherto supposed insoluble nature, but by means of oxalic acid
(whether obtained by the usual process of mixing or distilling saccharine matter,
in combination with nitric acid or from vegetable or other substances con-
taining oxalic acid, or from combinations of oxalates, whether metallic, earthy,
or alkaline) we obtain the above perfect solution of the Prussian blue, which
is applicable to dyeing, colouring, or staining in the various manufactures of
woollens, silks. linen. cotton, paper and such other substances 'as are required
to be dyed or stained, and which solution is also available to the purposes
of writing, or forming a writing fluid or ink to be used with "steel, quill, or
other pens.
Our third improvement, consisting in a peculiar manner f treating the
colouring matter of cochineal or of lac dye with other matter's for the purpose
of converting them into a red solution or dye, is effected by dissolving in boiling
water a quantity of common soda potash or carbonate of aminonia, to which is
to be added at intervals twice its weight of crude argol in powder. When the
effervescence arising from this combination has ceased we pour off the solution
or filter it from the insoluble matter; to this we add. by measure, half the
quantity of oxalate of alumina or oxala-phosphate of allumina, which we
prepare by adding to precipitated alumina or phosphate of alumina in a damp
state as much oxalic acid as will dissolve it. Into this mixture we put.
when cold, as much cochineal, first bruised or powdered, as will give it a fine
red colour, varying the quantity according to the shade of colour required,
and after letting it stand for the space of forty-eight hours we strain it off
for use.

page_text: Our fourth improvement (viz) combining carbonaceous matters with the
previously described solution of Prussian blue. or any colours, so as to form a
writing fluid or ink. 'which cannot be entirely effaced by chemical agents.
consists in dissolving resinous substances in solutions of alkali or alkaline salts
ly, means of heat, and adding to this solution fine lamp black or other car-
bonaceous matter. We take common carbonated alkali, or the potash or soda
of commerce, or ammonia, or some of the other alkaline salts will answer the
purpose, and mix it with a resinous matter, such as shel lac or rosin, about
equal parts by weight of each, altogether. We do not confine ourselves pre-
cisely to these proportions. We then add water according to the required
strength of the solution, and boil these until the resinous matter or a great
We then mix in a mortar the necessary
portion of it has become dissolved.
quantity of fine lamp black with this solution. and thereby produce a black
liquid, which black liquid may then be mixed with the Prussian blue solution,
or other suitable coloured solutions, to form an indelible ink. Such colouring
matter as is soluble in alkali will mix best with this composition.
In conclusion, we desire it to be understood, that we do not claim any of the
apparatus or machinery described, nor the calcination of animal matters in close
vessels. But we do claim the method of obtaining a product of prussiate of
potash or soda from the gases evolved from the distillation of animal matters,
or any other matters that yield azote and carburetted hydrogen, such, for
instance, as coal, by means of passing those gases direct into a mass of alkali
in a state of ignition, and into a solution of alkali contained in separate vessels,
either closely, or, distinctly connected with the distillatory apparatus.
Secondly, we do not claim the use of acids for the purpose of brightening
or improving the colour of Prussian blue in the ordinary manner, but we do
claim the use of strong acids for the purpose of digesting dry Prussian blue of
commerce, in order to render it more easily soluble in the oxalic acid than it
would be without such digestion.
And we further claim the use of oxalic acid, however obtained, as a solvent
for Prussian blue generally, but more especially as a final process for making a
perfect solution of. the Prussian blue which has been prepared and digested in
the manner above described.
Thirdly, we claim the application of oxalate or super-oxalate of alumina or
oxala-phosphate of alumina, in combination with the other materials described,
for the purposes of making a red solution for writing, staining. or colouring.
And,
Fourthly, we claim the combining or mixing of carbonaceous matters with
saline and alkaline solutions of resinous matter for the purpose of mixing with

page_text: such matters, we have been advised to alter and amend our said Title by
putting in the word "more" before the words "applicable to Dyeing,
Staining, and Writing," (that is to say,). we wish the Title of our said Patent
to be as follows: "Certain Improvements in Manufacturing Colouring Matter,
and Rendering certain Colour or Colours more applicable to Dyeing, Staining,
and Writing;" and for these several reasons aforesaid, we, the said Henry
Stephens and Ebenezer Nash, do hereby make the following alteration of
part of the Title of our said Invention, and for this reason, namely, in
order to make the same consistent with what our Specification will de-
scribe our said Invention to be when such alteration as aforesaid shall
have been entered (that is to say,) we insert the word "more" before the
words "applicable to Dyeing, Staining, and Writing" in the said Title of our
said Patent.
In witness whereof, we have hereunto set our hands, this Twenty-second
day of September, in the year of our Lord One thousand eight
hundred and thirty-seven.
HENRY STEPHENS.
EBENEZER NASH.
10 the Clerk of the Patents.
This is to certify that Henry Stephens, of Charlotte Street, in the Parish
of Saint Marylebonne, in the County of Middlesex, Gentleman, and Ebenezer
Nash, of Buross Street, in the Parish of Saint George in the East, and
County of Middlesex, Tallow Chandler, have applied to me for leave to enter
with you the above Memorandum of Alteration in the Title of their Invention,
for which Letters Patent were duly granted to them under the Great Seal of
Great Britain, bearing date at Westminster, the Eighteenth day of April now
last past; and on duly considering the said application, and hearing the parties
thereon, and no valid objection having been made to the said application, I
have accordingly allowed the same, and you are hereby authorized and directed
to stile the above-written alteration in the Title of their Patent, pursuant to
the Statute passed in the 5th & 6th years of the reign of His late Majesty
William the 4th, entitled An Act to amend the Law touching Letters
Patent for Inventions.
Dated this 22d day of Sentember 1837

page_text: AND BE IT REMEMBERED, that on the Twenty-sixth day of September,
in the first year of the reign of Her Majesty Queen Victoria, the said
Henry Stephens and Ebenezer Nash came before our said Lady the Queen in
Her Chancery, and acknowledged the Instrument aforesaid, and all and every
thing therein contained and specified, in form above written. And also the
Instrument aforesaid was stamped according to the tenor of the Statute made
in the fifty-fifth year of the reign of His late Majesty King George the
Third.
Inrolled the Twenty-eighth day of September, One thousand eight
hundred and thirty-seven.