AN IMPROVED PROCESS FOR THE REVIVIFICATION AND RECOVERY OF THE POTASH, SODA, AND ORGANIC COM- POUNDS REMAINING IN LYES AND SOAPS AFTER THEY HAVE BEEN USED FOR THE TREATMENT OF WOODY AND OTHER FIBRE AND FABRICS
Year: 1871

page_text: ETTERS PATENT to Thomas James Smith, of the Firm of Robertson,
Brooman, and Company, of 166, Fleet Strect, in the City of London,
Patent Agents, for the Invention of "AN IMPROVED PROCESS FOR THE
REVIVIFICATION AND RECOVERY OF THE POTASH, SODA, AND ORGANIC COM-
POUNDS REMAINING IN LYES AND SOAPS AFTER THEY HAVE BEEN USED FOR THE
TREATMENT OF WOODY AND OTHER FIBRE AND FABRICS."-A communi-
cation from abroad by Cyprien Marie Tessié du Motay, of Paris,
France.
Sealed the 22nd December 1871, and dated the 3rd July 1871.
PROVISIONAL SPECIFICATION left by the said Thomas James Smith at
the Office of the Commissioners of Patents, with his Petition, on
the 3rd July 1871.
I, THOMAS JAMES SMITH; of the Firm of Robertson, Brooman, and
5 Company, of 166, Fleet Street, in the City of London, Patent Agents,
do hereby declare the nature of the said Invention for "AN IMPROVED
PROCESS FOR THE REVIVIFICATION AND RECOVERY OF THE POTASH, SODA, AND

page_text: ORGANIC COMPOUNDS REMAINING IN LYES AND SOAPS AFTER THEY HAVE BEEN USED
FOR THE TREATMENT OF WOODY AND OTHER FIBRE AND FABRICS," to be as
follows:-
--
The potashes and sodas employed in a caustic state or as carbonates in
the boiling down of wood, straw, and other fibrous and textile substances
of a vegetable origin change their condition and become transformed
into resinates and ulmates of the same bases which no longer possess a
detersive or cleansing action, and are therefore thrown aside as possessing
no value. This is also the case with the alkalies and fatty matters
contained in the lyes and washes which have been employed for cleaning
purposes in the treatment of wool and finishing of silk.
This Invention consists, 1st, in transforming by a new method the
ulmates and resinates of potash or soda produced during the boiling of
woody and textile substances into carbonates or oxides of potassium or
sodium.
2ndly. In applying the same method to the lyes and soaps which have
been used for the cleansing of wool and the glossing of silk in order to
recover completely the alkalies and fatty bodies which are combined
therewith. When lyes or soaps which have been used for boiling
woody matters and textile materials, or for the cleansing of wool or
glossing of silk, are to be operated upon, bicarbonates of lime, magnesia,
or baryta, are caused to act upon them. The bicarbonates, which can
only exist in the presence of a continuous current of carbonic acid, are
produced in the midst of the liquid upon which they are to act. The
atomic quantities employed in order to produce insoluble soaps by
double decomposition by means of the bicarbonates vary with the
indetermined proportions of resins or fatty acids which contain the
lyes or soaps submitted to treatment; but in all cases they should be in
proportion to the equivalents of the resins or fatty acids to be saturated.
A chemical analysis of these lyes and soaps should therefore be made
before each treatment. The bicarbonates mentioned form by double
decomposition insoluble terrous resinates, ulmates, olcates, margarates,
stearates and soluble alkaline bicarbonates. The soluble salts are
separated by filtration or decantation, the alkaline bicarbonates are
raised to the boiling point, which removes the excess of carbonic acid,
and restores them to the state of carbonate, or they are boiled with lime
in order to return the potash and soda to the caustic state.

page_text: The insoluble salts are treated with any mineral acid which isolates :
and permits the recovery of either the resins or the fatty bodies com--
mercially valuable. The quantity of mineral acid employed in order to
decompose the insoluble salts thus generated is determined by the
amount of the base which these salts contain. When the sodas and:
potashes which have been used for the boiling down of certain woods or
other woody bodies not very rich in resin are from their richness. in.
alkali not readily revivified by the action of the soluble bicarbonates.
of lime, magnesia, or baryta, which are dissolved in the liquid, the
purification of these sodas and potashes is completed by the addition
of hydrate of baryta to the alkaline lyes to be revivified. Before:
employing the caustic baryta the lyes are to be treated previously by
the bicarbonates of lime, magnesia, or baryta, are decarbonated by lime.
The quantity of lime employed for this decarbonization is in proportion
to the quantity of alkaline carbonates contained in the liquids to
caustify, and is determined in each operation by a previous analysis.
The decarbonated baryta is then added to the lyes; it unites at once
with the resinous and ulmic products, and forms with them an insoluble
compound. The potash or soda liquids then pass into the caustic state,
and thus revivified are ready to serve again for fresh operations.
I proceed to describe more particularly the complete treatment which
the resinous soaps or lyes proceeding from the action of soda or potash
upon woody or other bodies of a similar nature are for the purposes
aforesaid made to undergo, in order, 1st, to return the alkali which these
soaps contain to the caustic state; 2nd, to recover the resin which with
this alkali formed a soluble soap. The Inventor has found that if these
soaps be treated by a prolonged current of carbonic acid without
the addition of a terrous base the carbonic acid thus employed will
alone displace almost the whole of the hydrate of colophane, and this
colophane regenerated in the midst of the carbonates of soda or potash
can be caked by a temperature of 212° Fahrenheit, and be precipitated
in the bottom of the vessels containing the alkaline carbonate lyes.
In consequence when lyes containing resinous soaps are to be treated
the operation is as follows:-1st. A current of carbonic acid is made to
pass through these lyes until the hydrate of colophane appears in the
midst of the liquid in a cloudy condition. 2nd. At this moment the
temperature of the bath is raised to the boiling point, and the action of

page_text: the heat is prolonged until the coagulation and complete precipitation of
the regenerated resin in an oily form. 3rd. After having removed this
resinous oil the alkaline lyes almost wholly deprived of the resinous
compounds are decarbonized by lime. 4thly. To the lyes thus de-
carbonated and brought back to the caustic state I add after previous
analysis a small quantity of bydrate of baryta with the addition or not.
of hydrate of lime, in order to precipitate it to the state of insoluble
soap any little particles of resin which may have escaped the principal
reaction. Lastly. The insoluble baryta soap thus produced is separated
from the caustified liquid by filtration or decantation.
SPECIFICATION in pursuance of the conditions of the Letters Patent,
filed by the said Thomas James Smith in the Great Scal Patent
Office on the 3rd January 1872.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, THOMAS
JAMES SMITH, of the Firm of Robertson, Brooman, and Company, of
166, Fleet Street, in the City of London, Patent Agents, send grecting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Third day of July, in the year of
our Lord One thousand eight hundred and seventy-one, in the thirty-
fifth year of Her reign, did, for Herself, Her heirs and successors, give
and grant unto me, the said Thomas James Smith, Her special licence
that I, the said Thomas James Smith, my executors, administrators,
and assigns, or such others as I, the said Thomas James Smith, my
executors, administrators, 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 "AN IMPROVED PROCESS
FOR THE REVIVIFICATION AND RECOVERY OF THE POTASH, SODA, AND ORGANIC
COMPOUNDS REMAINING IN LYES AND SOAPS AFTER THEY HAVE BEEN USED FOR THE
TREATMENT OF WOODY AND OTHER FIBRE AND FABRICS," (a communication
to me from abroad by Cyprien Marie Tessié du Motay, of Paris, France,)
upon the condition (amongst others) that I, the said Thomas James

page_text: Smith, 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 Scal Patent Office within six calendar months next and
immediately after the date of the said Letters Patent.
NOW KNOW YE, that I, the said Thomas James Smith, 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 the recovery by an improved process
of the alkalies and organic compounds remaining in lycs and soaps and
their solutions after they have been used in manufacturing processes,
such as are herein-after referred to.
Soda lye is now very largely used for boiling wood, straw, and other
woody matters to obtain a fibre suitable for the manufacture of paper;
potash lyc may be used in the same way. The alkali dissolves resinous
and other matters out of the wood or woody material, and heretofore in
order to render the alkali fit to be again used the lye has been evaporated
and the resin and other organic matters have been then burnt out. In
this process the evaporation of the lye is troublesome and costly and
the resinous matter is lost. By the treatment of these or similar lyes
according to this Invention evaporation is rendered unnecessary and the
resin is recovered. Again it is well known that soap is used on a large
scale for cleansing wool and in the treatment of silk and for many
other purposes.
By the treatment of such waste waters according to this Invention the
alkali and fatty matters they contain are recovered. The lyes or soaps
left in such waste waters after they have been used are acted upon with
bicarbonate of lime, magnesia, or baryta. These bicarbonates, which
can only exist in the presence of a continuous current of carbonic acid
or its equivalent, are produced in the midst of the liquid upon which
they are to act. The atomic quantities employed in order to produce
insoluable soaps by double decomposition by means of bicarbonates vary
with the undetermined proportions of resins or fatty acids which the
lycs or soaps submitted to treatment contain, but in all cases they
should be in proportion to the equivalents of the resins or fatty acids

page_text: to be saturated. A chemical analysis of these lycs and soaps should
therefore be made before cach treatment. The bicarbonates mentioned
form by double decomposition insoluble terrous resinates, ulmates,
oleates, margarates, and stearates, and soluble alkaline bicarbonates.
The soluble salts are separated by filtration or decantation, the alkaline
bicarbonates are raised to the boiling point, which removes the excess
of carbonic acid and restores them to the state of carbonate, or they are
boiled with lime in order to return the potash and soda to the caustic
state.
The insoluble salts are treated with a mineral acid which isolates and
permits the recovery of either the resins or the fatty bodies commercially
valuable. The quantity of mineral acid employed in order to decompose
the insoluble salts thus generated is determined by the amount of the
base which these salts contain. When the sodas and potashes which have
been used for the boiling down of certain woods or other woody bodies
not very rich in resin are from their richness in alkali not readily
revivified by the action of the soluble bicarbonates of lime, magnesia,
or baryta which are dissolved in the liquid, the purification of these sodas
and potashes is completed by the addition of hydrate of baryta to the
alkaline lyes to be revivified. Before employing the caustic baryta the
lycs treated previously with the bicarbonate of lime, magnesia, or baryta
are decarbonated by lime. The quantity of lime employed for this
decarbonization is in proportion to the quantity of alkaline carbonates
contained in the liquid to caustify, and is determined in each operation
by a previous analysis. The decarbonated baryta is then added to the
lycs; it unites at once with the resinous and ulmic products and forms
with them an insoluble compound. The potash or soda liquids are now
in a caustic state, and thus revivified are ready to serve again for fresh
operations.
I will now proceed to describe a modification of the process which is
more applicable to the treatment of the resinous soaps or lyes proceeding
from the action of soda or potash upon woody or other bodies of a
similar nature. The lye is treated with currents or a prolonged current
of carbonic acid gas without the addition of a terrous base, the carbonic
acid thus employed will alone displace almost the whole of the hydrate of
colophone or resin, and this colophone is precipitated in the midst of
the liquid containing carbonates of soda or potash in solution, and can

page_text: be caked by heating the liquid to 212° Fahrenheit, when it falls to the
bottom of the vessels containing the alkaline carbonate lyes.
The operation is as follows:-1st. A current of carbonic acid gas
obtained from any convenient source is made to pass through the lyes
until the hydrates of colophone appears in the midst of the liquid in a
cloudy condition; this operation is continued until by the examination
of samples it is ascertained that the action is complete. 2ndly. At this
moment the temperature of the bath is raised to the boiling point,
and the action of the heat is prolonged until the coagulation and
complete precipitation of the regenerated. resin. 3rdly. After having
removed the resinous matter the alkaline lyes almost wholly deprived
of the resinous compounds are rendered caustic by lime. 4thly. To the
lyes thus decarbonated and brought back to the caustic state I add
after previous analysis a small quantity of hydrate of baryta sufficient
to combine with the remaining resinous matter in order to precipitate
to the state of insoluble soap any little particles of resin which may
have escaped the principal reaction. Lastly. The insoluble baryta
soap thus produced is separated from the caustified liquid by filtration
or decantation.
In place of using baryta as above set forth to obtain a more complete
precipitation of the resin and other matters with which the alkali is
charged, sulphide of sodium may be employed. It is added at the end
of the first stage of the operation, and the passage of carbonic acid gas
through the liquor is resumed and continued until the whole of the
sulphide is decomposed with the liberation of sulphuretted hydrogen and
the formation of carbonate of soda. The quantity of sulphide employed
may be varied, but in practice it is convenient to add sufficient to make
good the loss of alkali from the previous boiling.
The use of sulphide of sodium in this manner is described in the
Provisional Specification filed by me with my application for Letters
Patent made on the First day of January 1872, No. 2, and forms no part
of the Invention claimed under this Patent. It is here mentioned only
for the purpose of indicating the best means with which I am at present
acquainted for the entire treatment of lyes before they are re-used.
I have referred more particularly to the employment of carbonic acid
gas as the agent for decomposing the resinates and ulmates in the lyes,
but other gases having the properties of combining with the alkali

page_text: and afterwards when the resin is separated and lime is added of again
liberating the alkali can be employed in lieu of carbonic acid or in
combination therewith.
Having thus described the nature of the said Invention, and in what
manner the same is to be performed, I declare that I claim,-
Firstly. The improved process for the revivification and recovery of
the potash, soda, alkalies, soaps, fats, or other bodies from lyes or washi
waters by the employment of carbonic acid gas or gases that will act
in an equivalent manner, substantially as described.
Secondly. I claim the employment of the soluble bicarbonates of
lime, magnesia, or baryta, as well as of the hydrate of baryta in the
recovery of the potash, soda, and organic compounds contained in lyes
and wash waters; substantially as described.
In witness whereof, I, the said Thomas James Smith, have here-
unto set my hand and seal, this Second day of January Onc1
thousand eight hundred and seventy-two..