A NEW APPLICATION OF CERTAIN FLUIDS POR MANUFACTURING EXTRACTS APPLICABLE TO THE PROCESSES OF DYEING, PRINTING, AND TANNING, AND IN THE APPARATUS CONNECTED THEREWITH
Year: 1851

page_text: TO ALL TO WHOM THESE PRESENTS SHALL COME, I, FREDERICK
CRACE CALVERT, of Manchester, in the County of Lancaster, Professor of
Chemistry and Analytical Chemist, send greeting.
WHEREAS Her present most Excellent Majesty Queen Victoria, by Her
Letters Patent under the Great Seal of the United Kingdom of Great
Britain and Ireland, bearing date at Westminster, the Twelfth day of June
now last past, did, for Herself, Her heirs and successors, give and grant unto
me, the said Frederick Crace Calvert, my exors, admors, and assigns, Her
especial licence, that I, the said Frederick Crace Calvert, my exors, admors,
and assigns, or such others as I, the said Frederick Crace Calvert, my exors,
admors, and assigns, should at any time agree with, and no others, from time
to time and at all times during the term of years therein expressed, should
and lawfully might make, use, exercise, and vend, within England, Wales,
and the Town of Berwick-upon-Tweed, my Invention of "A NEW APPLICATION
OF CERTAIN FLUIDS POR MANUFACTURING EXTRACTS APPLICABLE TO THE PROCESSES OF
DYEING, PRINTING, AND TANNING, AND IN THE APPARATUS CONNECTED THEREWITH;"
in which said Letters Patent is contained a proviso, obliging me, the said
Frederick Crace Calvert, by an instrument in writing under my hand and seal,
particularly to describe and ascertain the nature of my said Invention, and in
what manner the same is to be performed, and to cause the same to be enrolled
in Her said Majesty's High Court of Chancery within six calendar months
next and immediately after the date of the said recited Letters Patent, as in

page_text: and by the said Letters Patent, reference being thereunto had, will more
fully and at large appear.
NOW KNOW YE, that in compliance with the said proviso, I, the said
Frederick Crace Calvert, hereby declare that the nature of the first part
of my said Invention consists in employing certain volatile fluids never before
used for that purpose for manufacturing extracts to be used in dyeing,
printing, and tanning. It is essential that these fluids should possess the two
following properties, first, they should be easily transformable into vapour,
and recondensible with facility; secondly, they should be enabled by their
chemical composition, to dissolve with facility the coloring or tanning matters
or principles from the substances in which they are contained, and also resins
and the resin of gum resins. The fluids which I have employed, and which
I consider to be most suitable, are rich in carbon and hydrogen, or are com-
posed entirely of carbon and hydrogen, and are the impure hydrate of oxide
of methyle, or what is usually called wood naptha, pyroligneous spirit, acetone,
or the hydrate of oxide of mesithyle, turpentine, camphine, those volatile oils
which are obtained by the destructive distillation of resins, the volatile oil
obtained by the destructive distillation of shale coal, and any other bituminous
shale or schist, also the volatile carburetted hydrogens obtained by the distil-
lation of coal tar, which are usually known by the name of coal or mineral
naptha; also those which may be obtained from the distillation of vegetable
tars, and from peat or bog, or from tar and oil obtained from peat and bog;
lastly, alcohol and ethers, such as the hydrate of oxide of ethyle, the acetate of
the oxide of ethyle or other ethers.
The nature of the next part of my Invention consists in the apparatus which
I employ in manufacturing such extracts, and will be best understood by the
following description, and by reference to the Drawings hereto annexed:-
Fig. 1 is a side elevation of the apparatus; Fig. 2 is a plan view; and
Fig. 8 is an end elevation of the same. In these views M is a boiler, which
is furnished with a casing, and is heated by steam or other suitable means.
To the lid of the boiler is attached a long tube N surrounded by a casing, the
object of which is to have a circulation of steam between the tube and the
casing to keep the vapour of the volatile fluid as it rises from the boiler N from
condensing before it has reached the condenser O. From this condensor the
volatile fluid runs through the pipe O' into a receiver P, where it may be kept
until required; from the receiver P the liquid is conducted by the tubes P¹,
into one of the two large boxes R, which are intended to be used alternately,
as a considerable saving of time will be effected by the alternate use of each;
these boxes are lined with copper and divided into compartments by the plates

page_text: R', each of which is one-third of the height of the box. Into the boxes R is
put a certain quantity of the substance containing the colouring or tanning
matter or principle, which substance is either dry or moist, having been
moistened with water or with solutions of fixed alkalies, such as potash, soda,
or ammonia, or with alkaline carbonates, or bicarbonates, phosphates, borates,
and sulphates of soda, silicates of soda and potash, stannates of soda or potash,
lime, carbonate of lime, baryta, strontia, and their carbonates, magnesia and its
carbonates, and oxide of lead. The above alkalies and substances presenting
an alkaline reaction, may also be mixed in a dry state with the substances con-
taining the coloring and tanning matter or principle previous to their being
placed in the boxes R. I find it sometimes necessary to treat the substance
containing the coloring or tanning matter or principle previously to putting
them into the boxes R, by washing or macerating them with one of the above
named alkalies or their salts, having an alkaline reaction dissolved in water.
The boxes R are provided below with steam pipes R, which are covered by a
false bottom answering the purpose of a filter, as seen best in Fig. 1, in which
view one of the boxes is shewn partly in section. The upper parts of the boxes
are provided with cones R³, which serve as heads of stills, and communicate by
two main pipes R³, with a separate condenser T; each compartment of the
boxes R is provided with a man-hole on the top, see Fig. 2, by which the sub-
stances containing the coloring or tanning matter or principle, are introduced,
and with an opening near the false bottom, by which they are afterwards with-
drawn. In beginning the operation, the volatile fluid to be used is put into
the receiver P, from whence it is let down into one of the boxes R upon the
substance from which the coloring or tanning matter or principle is to be
extracted, and which substance is then either dry or moist, or mixed with one
of the substances above enumerated, according to the nature of the substance
to be operated upon and the effect desired. The fluid is there allowed to
macerate the contents of the boxes for a certain number of hours, or to
percolate through them according to circumstances, or if desired, it may be
brought into the box R in a state of vapour, either direct from the boiler M or
otherwise, to be there condensed and to act directly on the substances contained
therein. The fluid is then allowed to pass into a recipient S, through the
pipes R, and from thence into the boiler or evaporating vessel M, through the
pipe S'; the fluid is then volatilized, and leaves behind the tanning or coloring
matter or principle, and the resin or gum resin, with which the coloring or
tanning matter or principle is generally mixed or combined, the volatile fluid
arrives again in the boxes R, either in a liquid state, if previously condensed
in O, or in a state of vapour, if brought direct from the boiler M. The fluid

page_text: again removes a certain quantity of coloring or tanning matter or principle from
the substances in the box R, and when sufficiently impregnated, it is allowed to
pass through the recipient S into the boiler M; these successive operations are
to be repeated as often as it is deemed necessary. Near the end, and above the
receiver P, is placed a vessel P, in which is contained a hollow conical vessel
P2, terminating in a tube reaching nearly to the bottom of the vessel P. From
the summit of the conical vessel P' a pipe P' is carried, having branches com-
municating with the receiver P, the boxes R, and recipient S. The object of
this apparatus is to prevent in a great measure the escape of the vapours of
the volatile fluid. 'On commencing operations, the vessel P is partly filled
with water, and when heat is applied to the boiler M, the air is chased by the
vapours of the volatile fluid through the pipe N, condensor O, and receiver P,
then through the pipe Ps, conical vessel P³, and through the water in the
vessel P, and the vapours of the volatile fluid which would otherwise escape
with the air, are retained by the water in the vessel P. The object of the
conical vessel P is that when absorption takes place owing to the cooling of the
boiler M, or from any other cause, the water from the vessel P enters into the
conical vessel P³, and remains there until again expelled by the air in its escape
from the apparatus as before described. In order to obtain that portion of the
volatile fluid which has remained in the exhausted or partially exhausted sub-
stances contained in the boxes R, it is necessary to admit water into the said
boxes; and after the water has been left a sufficient time to mix with the
remaining volatile fluid and coloring or tanning matter or principle, it is
then allowed to pass through the recipient S into the boiler M, where heat is
applied, whereby the volatile fluids are separated from the water, and are
received into the receiver P through the condensor O; the extract thus
obtained is then drawn off through the tap W. Sometimes water may be
advantageously used more than once in the way above named. Heat is then
to be applied through the steam pipes R contained in the false bottom of the
boxes R to heat the mass of organic substances from which the coloring or
tanning matter or principle has been extracted, and if any of the volatile
fluids have remained mixed with or absorbed by the above-named exhausted
substances, they are driven through the still-heads R2 and pipes R³, above
mentioned into the condensor T; the refusè substance is then removed
through the openings near the bottom of the boxes R, and the apparatus
is ready for a new operation. It may, in some cases be found advantageous to
perform the operation of boiling up the exhausted or partially exhausted
substances contained in the boxes R in a separate apparatus. When this
mode of operating is adopted, the boxes R can be made with only one man-

page_text: hole for the admission of the substances to be operated upon, and the still-
heads R, pipes R³, and condensor T would be dispensed with. When sumac
is the substance from which an extract is to be made, I prefer the use of wood
naphtha as the volatile fluid, by the agency of which the extract is made. The
sumac, after being moistened with water, is placed in each of the boxes R, being
evenly distributed in the several compartments of the said boxes R, and the
naphtha put into the receiver P is let down into the boxes R, and remains there
until it has extracted or dissolved a portion of the tanning matter or principle,
and also a portion of the resin of the sumac. The attendant, by opening the
tap in the pipe R', then allows the naphtha to flow from both the boxes R into
the recipient S, which is divided into two compartments; the contents of one
of these compartments is then conducted to the boiler M by the pipe S¹. The
attendant now admits a fresh supply of naphtha from the receiver P into the
boxes R, and while this naphtha is operating on the sumac, as before described,
heat is applied to the boiler M, and the naphtha in the boiler becoming vola-
tilized, passes off through the tube N into the receiver P, leaving the extract
of sumac in the boiler, from whence it may be drawn by the tap W. The
naphtha contained in the second compartment of the recipient S, is then
allowed to run into the boiler, where it is volatilized as before, and is collected
in the other compartment of the receiver P, the extract remaining in the boiler
being drawn off at the tap W as before. The naphtha from the boxes R is
then let off into the recipient. S, and the naphtha from the receiver P is
allowed to run into the boxes R as before described, and the operations are
repeated as often as is found necessary. When the sumac has become nearly
exhausted, instead of naphtha water, is admitted into the boxes R from
the vessel L, in order to obtain a portion of the tanning matter or principle,
and of the naphtha remaining in the sumac; this water passes into the
boiler M where the naphtha is expelled from it, and the extract withdrawn as
before described. The extract thus last obtained may be mixed with the
extracts previously obtained, either with or without an additional quantity of
water as may be found desirable, and the whole is allowed to settle and clarify
to render it fit for use. Water is again let on to the sumac in the boxes R,
and the heat applied through the steam pipes R³, until all the remaining portion
of naphtha is expelled through the still-heads R* and pipes R³, and condensed
in the condenser T. The naphtha remaining in the apparatus is ready for
treating the next charge of sumac. The quantity of naphtha to be employed
at one operation, depends in a great measure upon the quality of the sumac to
be operated upon; but any practical chemist will soon discover the proper
proportions, and also which volatile fluids are best adapted for manufacturing

page_text: extracts from other substances containing coloring and tanning matters or
principles. Or, in treating substances containing tanning matter or principle,
I sometimes employ, instead of the apparatus above described and a volatile
fluid, simply an alkali or a substance presenting an alkaline reaction. When
this method is adopted, the substances containing the tanning matter or prin-
ciple are treated with an alkaline solution by maceration or percolation. This
solution may be used either with or without the aid of heat. Although these
operations can be conducted in open vessels, I prefer to make them in closed
vessels or in partly-exhausted vessels, as it is well known that tannin or tanning
matter and gallic or pyrogallic acid undergo rapid oxidation or destruction
when under the influence of alkalies by absorbing the oxygen of the atmo-
sphere. It is also in some cases advantageous to add to these extracts a
sufficient quantity of an organic or mineral acid, to neutralize the quantity of
alkali, alkaline earths, or their carbonates, and to give a slight acid reaction to
the solution, in which the above-mentioned substances, presenting an alkaline
reaction have been employed.
Having now described the nature and particulars of my Invention, I wish it
to be well understood that I do not confine myself to the particular form of
apparatus herein-before described; but what I wish to secure the exclusive use
of is an apparatus so constructed that any of the above-named volatile agents
employed to extract the colouring or tanning matters or principles are made to
pass through the substances containing the same, and in passing to extract a
portion of the colouring or tanning matter or principle, from which they are
liberated by the application of heat. The agent employed being volatilized
rises through a tube or aperture to be condensed, and then passes through the
substances to be acted upon, the operations being repeated as often as
necessary.
And I claim, first, the application of the above-named volatile fluids for the
manufacture of extracts from substances containing colouring and tanning
matters or principles, which extracts are applicable in the processes of dyeing,
printing, and tanning.
Secondly, I claim the apparatus herein-before described for the manufacture
of extracts applicable to dyeing, printing, and tanning, by which apparatus the
volatile fluids I have enumerated, or any others possessing the same or similar
qualities, are volatalized (leaving the colouring or tanning matter or principle
in the evaporating vessel), and then condensed and employed in the manner
herein-before described.
Thirdly, I claim the use of the above-named alkalies and substances having
an alkaline reaction when mixed with substances containing colouring or

page_text: tanning matters or principles previous to subjecting them to the action of
volatile fluids, as above described.
Fourthly, I claim the manufacturing of extracts from substances containing
tanning matters or principles by the agency of alkalies or substances presenting
an alkaline reaction.
And this my Invention being to the best of my knowledge and belief entirely
new and never before used within that part of Her said Majesty's United
Kingdom of Great Britain and Ireland called England, Her Dominion of
Wales, and Town of Berwick-upon-Tweed, I do hereby declare this to be my
Specification of the same, and that I do verily believe this my said Specification
doth comply in all respects fully and without reserve or disguise with the
proviso in the said herein-before in part recited Letters Patent contained,
wherefore I do hereby claim to maintain exclusive right and privilege to the
said Invention.
In witness whereof, I, the said Frederick Crace Calvert, have hereunto
set my hand and seal, this Tenth day of December, in the year of our
Lord One thousand eight hundred and fifty-one.
FREDERICK (L.s.) CRACE CALVERT.
AND BE IT REMEMBERED, that on the Tenth day of December, in the
year of our Lord 1851, the aforesaid Frederick Crace Calvert came before
our said Lady the Queen in Her Chancery, and acknowledged the Speci-
fication aforesaid, and all and every thing therein contained and specified, in
form above written. And also the Specification aforesaid was stamped
according to the tenor of the Statute made for that purpose.
Enrolled the Eleventh day of December, in the year of our Lord One
thousand eight hundred and fifty-one.