Improvements in or relating to the Treatment of Vegetable Materials to Fit them for the Manufacture of Paper, Pasteboard, Threads, Tow, or other like Objects.
Year: 1887

page_text: Date of Application, 20th Sept., 1887
Complete Left, 14th June, 1888
Complete Accepted, 20th July, 1888
Improvements in or relating to the Treatment of Vegetable
Materials to Fit them for the Manufacture of Paper, Pasteboard,
Threads, Tow, or other like Objects.
I PAUL EMILE EDMOND PESIER, of 1. Boulevard St. Denis, Paris, France, Manu-
facturing Chemist, do hereby declare the nature of this invention to be as
follows:-
This invention relates to the treatment of vegetable materials in such manner as to
fit them for the manufacture of paper paste-board threads tow and other like objects, and
it consists in submitting them to a succession of operations the combination of which
constitutes a rational manufacturing method by which vegetable fibres are obtained
in a purified state with a maximum production and quality. These operations are
divided as follows:-
1. Alkalino-caustic lixiviation by maceration in the open air.
2. Successive diffusions in the open air in alkalino-caustic liquids the strengths of
which are regulated with the aid of an alkalimetric control and which become enriched
progressively in the humid way by the excess of the alkalino-caustic agent, of a higher
strength, absorbed by the material under treatment in the course of the initial mace-
ration. Tending thus to attain gradually the alkalino-caustic strength of the maceration
these liquids are successively and mathematically transferred from one diffusing vessel
to another to the macerating vessels where by a slight chemically regulated addition
of the alkalino-caustic agent at a high degree they proportionately replace in strength
and volume the portion of the macerating agent which has entered into combinations
or been taken up by absorption.
3. Hot treatment or separation by boiling of the matters in combination not left in
the cold diffusers and still present in the midst of the material under treatment.
4. Chemical defecation of the waste waters and recovery of the organic matters con-
tained in these waters.
The whole being followed or not by the utilization of the alkalino organic residues
from the macerators and diffusers as saponifiable products.

page_text: The material to be treated is put to macerate in an alkalino-caustic lye capable of
titrating up to 5000 alkalimetric degrees per litre, say 50 degrees Gay Lussac,
according to the nature of the material. The alkalimetric strength of the lye is the
principal point in the operations and account should be taken of the nature of the
material, the ambiant temperature and the duration of the maceration. To ascertain the
proper strength for the lye it is necessary before commencing full work to make
experiments for each description of plant or fibrous material to be treated. Maceration
may be considered perfect when on the material being taken out several times and allowed
to drain for an equal length of time and being each time returned to maceration for
an equal length of time it is found after several repetitions that the volume and the
strength of the lye have become invariable. The temperature being practically the
same during the limited periods, the material tested being taken from a portion of
identical nature and the duration of each operation be maintained for an equivalent
tire, therefore as the material absorbs no more liquid it is impregnated to saturation
and the alkalino-caustic agent has penetrated all its parts. Therefore also as the
alkalino-caustic strength remains stable the chemical action is no longer exerted and
all possible alkalino-organic combinations have been effected and completed. By this
double test the proper strength and duration of the macerating treatment are deter-
mined. By these tests the quantity of the alkalino-caustic agent which has entered
into combination or been absorbed by the material is ascertained. It is then indis-
pensable in a manufacturing and economical point of view to separate the combined
products both from the material itself and from the impregnating alkalino caustic
liquids and to recover the greatest possible quantity of the latter which have preserved
all their active value.
These objects are attained by the successive diffusions. The diffusions are conducted
as follows:-
The amount of the alkalino-caustic agent which has entered into combination is
ascertained by deducting from the product of the multiplication of the number of
initial litres of the macerating lye by the alkalimetric degree of this lye, that of the
multiplication of the number of litres found in the macerator at the end of the test
operations by the alkalimetric degree of this lye when the operations are finished.
This result which enables the amount of the final expenditure of the alkalino-caustic
agent by combinations to be exactly ascertained is the function of the successive
degrees of strength at which the liquids of the diffusers in the system should be
fixed. These diffusion liquids should be titrated gradually diminishing by an equal
number of alkalimetric degrees starting from the first of them, the strength of which
should be lower than that of the macerating liquid when the maceration is finished :
the difference of strength to be established between the diffusers should be equal to
the number of alkalimetric degrees that it is decided to lose at the end of the
operations.
Example. If after having macerated for 12 hours 100 kilogrammes of the material
under treatment,

page_text: treatment can be passed successively from one vessel to another with or without the
employment of cages with compartments; or it can be submitted to the diffusing and
macerating actions in the same vessel by gradually changing the macerating and
diffusing baths by any of the known modes of circulating liquids but always pro-
viding for the descending order of their alkalino-caustic strengths.
It will be understood that in all cases the liquids held in the matter under treat-
ment being richer in soluble alkaline salts and denser than the liquids in which they
are immersed equilibrium will tend to be established between them, and that thus the
recovery will be effected by virtue of a regular and natural law up to the minimum
loss decided upon; it is simply a question of the number of vessels at the will of the
operator it will also be understood that the material having during the maceration
absorbed and taken up the maximum of liquid that it can hold the volumes of liquid
contained in the successive vessels could not be sensibly modified.
Nevertheless, as on the one hand the macerating liquids are impoverished in strength
by the entrance, into alkalino-organic combination of a part of the alkalino-caustic
agent and diminished in volume by the quantity absorbed and taken up by the
macerated material; and as on the other hand the diffusing liquids become progres-
sively enriched in strength by the addition of the soluble alkalino-caustic salts which in
the course of the diffusions the material under treatment gives up to them successively
and which it has taken from the macerator,-it is necessary to provido for com-
pensations in order to maintain regularity of the operations. These compensa-
tions are logically and easily obtained by means of the liquids as follows:-
A reserve vessel placed near the macerators and containing a sufficient quantity of
concentrated alkalino-caustic liquid at a higher degree of strength than the initial
degree of the macerators supplies these with the necessary elements for their reconsti-
tution in strength and volume. This vessel receives after each maceration a volume
of liquid equal to that which has been taken up by the material treated; this liquid is
supplied to it by the first diffuser. It is thus sufficient in order to maintain the
reserve at the high degree it ought to have to add thereto the proportionate quantity
of alkalino-caustic salts in the solid state.
It will be understood that in this way the reconstitution in strength and volume of
a macerator is always easy and well regulated. Besides, this operation links in
with the like regulation of the volumes and strengths of the diffusing vessels.
In short, the first diffuser having supplied a volume of liquid equal to that which the
macerated material has itself taken up, its level is reestablished by the immersion of
this material therein. But after the diffusion its alkalimetric strength will be heightened
by the addition of soluble alkalino-caustic-salts-of-a-high degree of strength which
this material has made.
In order to restore this first diffusing bath to its normal strength and to allow it to
furnish for the following operation the proper volume of liquid to the reserve,
immediately the first diffusion is finished this same volume of liquid is taken from
the second diffuser the strength of which has been established with a difference
absolutely the same as that which should exist between the strength of the macerator
at the end of the maceration and the first diffuser at the beginning of the operation.
This addition reestablishes by compensation the normal alkalimetric strength.
The total expenditure of alkalino-caustic salts can be easily calculated. It consists
of the difference between the initial alkalimetric strength of the macerating bath and
that of the same bath after maceration; and the final loss decided upon and fixed
beforehand.
The diffusions having been finished the material under treatment is transferred with-
out being washed and after simple draining into an agitating vessel in which it
receives a hot treatment with clear water. This boiling, repeated if necessary, has for
object to remove from it matters in combination or not combined and alkalino-caustic
salts which it has carried from the last diffuser. The duration of the boiling varies
from 1 to 2 hours according to the material treated.
It will be understood that there can be nothing absolute in these indications of
duration as the diversity of the materials and the nature of the waters necessarily

page_text: make it variable; but the termination of these operations is easily ascertained by
taking a small part of the boiled material and rinsing it in clear water.
The
appearance of the fibre, its whity-brown color and the facility with which it
separates on being rubbed by hand are indications that cannot mislead.
The boiling having been finished nothing further is required, if it is wished to
employ the raw fibre, than to thoroughly wash it. If on the contrary it is desired to
bleach it any ordinary bleaching operations can be followed.
The lye residues can be utilized by saponifying them; the operation is easy as the
residues are eminently fitted therefor. With this object the liquids after having been
allowed to settle are decanted; the magmas, compounds of the alkalino-caustie
matters arising from the combinations during the maceration, are deposited at the
bottom of the vessel and are collected to be saponified or sold to soap makers.
There is nothing more, as residues to be rejected than the waters from the boiling
operation the discharge of which into streams might be objectionable. They should
therefore be clarified. They are defecated by treatment with a slight excess of
ordinary hydrochloric acid of commerce. The organic matters precipitate and the
waters can then be run off into streams. The organic precipitates collected have a
value as they can be utilized in the manufacture of manure.
Dated this 20th day of Santambar 1887

page_text: Improvements in or relating to the Treatment of Vegetable
Materials to Fit them for the Manufacture of Paper, Pasteboard,
Threads, Tow, or other like Objects.
I PAUL EMILE EDMOND PESIER, of 1 Boulevard St. Denis, Paris, France, Manu-
facturing Chemist, do hereby declare the nature of this invention and in what manner
the same is to be performed, to be particularly described and ascertained in and by
the following statement :-
This invention relates to the treatment of vegetable materials in such manner as to
fit them for the manufacture of paper, pasteboard, threads, tow and other like objects,
and it consists in submitting them to a succession of operations the combination of
which constitutes a rational manufacturing method by which vegetable fibres are
obtained in a purified state with a maximum production and quality. These operations
are divided as follows:-
:-
1. Alkalino-caustic lixiviation by maceration in the open air.
2. Successive diffusions in the open air in alkalino-caustic liquids the strengths of
which are regulated with the aid of an alkalimetric control and which become
enriched progressively in the humid way by the excess of the alkalino-caustic agent,
of a higher strength, absorbed by the material under treatment in the course of the
initial maceration. Tending thus to attain gradually the alkalino-caustic strength of
the maceration these liquids are successively and mathematically transferred from
one diffusing vessel to another to the macerating vessels whereby a slight chemically
regulated addition of the alkalino-caustic agent at a high degree they proportionately
replace in strength and volume the portion of the macerating agent which has entered
into combinations or been taken up by absorption.
3. Hot treatment or separation by boiling of the matters in combination not
left in the cold diffusers and still present in the midst of the material under
treatment.
4. Chemical defecation of the waste waters and recovery of the organic matters
contained in these waters.
The whole being followed or not by the utilization of the alkalino-organic residues
from the macerators and diffusers as saponifiable products, or by the recovery of the
soda by the incineration of the magmas.
The material to be treated is put to macerate in an alkalino-caustic lye capable of
titrating up to 5000 alkalimetric degrees per litre, say 50 degrees Gay Lussac, accord-
ing to the nature of the material. The alkalimetric strength of the lye is the
principal point in the operations and account should be taken of the nature of the
material, the ambiant temperature and the duration of the maceration. To ascertain
the proper strength for the lye it is necessary before commencing full work to make
experiments for each description of plant or fibrous material to be treated. Maceration
may be considered perfect when on the material being taken out several times and

page_text: allowed to drain for an equal length of time and being each time returned to
maceration for an equal length of time it is found after several repetitions that the
volume and the strength of the lye have become invariable. The temperature being
practically the same during the limited periods, the material tested being taken from
a portion of identical nature and the duration of each operation being maintained fór
an equivalent time, therefore as the material absorbs no more liquid it is impregnated to
saturation and the alkalino-caustic agent has penetrated all its parts. Therefore also
as the alkalino-caustic strength remains stable the chemical action is no longer
exerted and all possible alkalino-organic combinations have been effected and com-
pleted. By this double test the proper strength and duration of the macerating
treatment are determined. By these tests the quantity of the alkalino-caustic agent
which has entered into combination or been absorbed by the material is ascertained.
It is then indispensable in a manufacturing and economical point of view to separate
the combined products both from the material itself and from the impregnating
alkalino-caustic liquids and to recover the greatest possible quantity of the latter
which have preserved all their active value.
These objects are attained by the successive diffusions. The diffusions are conducted
as follows-The amount of the alkalino-caustic agent which has entered into com-
bination is ascertained by deducting from the product of the multiplication of the
number of initial litres of the macerating lye by the alkalimetric degree of this lye,
that of the multiplication of the number of litres found in the macerator at the end
of the test operations by the alkalimetric degree of this lye when the operations are
finished. This result which enables the amount of the final expenditure of the alkalino-
caustic agent by combinations to be exactly ascertained is the function of the
successive degrees of strength at which the liquids of the diffusers in the system
should be fixed. These diffusion liquids should be titrated gradually diminishing by
an equal number of alkalimetric degrees starting from the first of them, the strength
of which should be lower than that of the macerating liquid when the maceration is
finished the difference of strength to be established between the diffusers should be
equal to the number of alkalimetric degrees it is decided to lose at the end of the
operations.
Example. If after having macerated for 12 hours 100 Kilogrammes of the material
under treatment
=
Thus there would be 150 litres at the final strength of 3,800° contained in the
macerated material, recoverable in the humid way by the aid of the diffusions. The
irrecoverable loss by combination would therefore only be 750,000°- (150 x 3800°)
570,000° 180,000°. In order to effect the diffusions in this case admitting that it
is decided at the end of the operations to have a loss of 200° per litre, 18 diffusing
vessels are necessary the liquids of which, of the same volume as the macerators,
would titrate in a descending scale of 200° between each of them from 3600°
to 200°..
As desired and according to the manufacturing requirements, the material under
treatment can be passed successively from one vessel to another with or without the
employment of cases with compartments; or it can be submitted the diffusing and
macerating actions in the same vessel by gradually changing the macerating and
diffusing baths by any of the known modes of circulating liquids but always providing
for the descending order of their alkalino-caustic strengths.
It will be understood that in all cases the liquids held in the matter under treat-
ment being richer in soluble alkaline salts and denser than the liquids in which they
are immersed equilibrium will tend to be established between them, and that thus the

page_text: recovery will be effected by virtue of a regular and natural law up to the minimum
loss decided upon; it is simply a question of the number of vessels at the will of the
operator; it will also be understood that the material having during the maceration
absorbed and taken up the maximum of liquid that it can hold the volumes of liquid
ontained in the successive vessels could not be sensibly modified.
Nevertheless, as on the one hand the macerating liquids are impoverished in strength
by the entrance into alkalino-organic combination of a part of the alkalino-caustic
agent and diminished in volume by the quantity absorbed and taken up by the
macerated material; and as on the other hand the diffusing liquids become pro-
gressively enriched in strength by the addition of the soluble alkalino-caustic salts
which in the course of the diffusions the material under treatment gives up to them
successively and which it has taken from the macerator, it is necessary to provide
for compensations in order to maintain regularity of the operations. These com-
pensations are logically and easily obtained by means of the liquids as follows:-
A reserve vessel placed near the macerators and containing a sufficient quantity of
concentrated alkalino-caustic liquid at a higher degree of strength than the initial
degree of the macerators supplies these with the necessary elements for their recon-
stitution in strength and volume. This vessel receives after each maceration a volume
of liquid equal to that which has been taken up by the material treated; this liquid
is supplied to it by the first diffuser. It is thus sufficient in order to maintain the
reserve at the high degree it ought to have to add thereto the proportionate quantity
of alkalino-caustic salts in the solid state.
It will be understood that in this way the reconstitution in strength and volume of
a macerator is always easy and well regulated. Besides, this operation links in with
the like regulation of the volumes and strengths of the diffusing vessels.
In short, the first diffuser having supplied a volume of liquid equal to that which
the macerated material has itself taken up, its level is reestablished by the immersion
of this material therein. But after the diffusion its alkalimetric strength will be
heightened by the addition of soluble alkalino-caustic salts of a high degree of strength
which this material has made.
In order to restore this first diffusing bath to its normal strength and to allow it
to furnish for the following operation the proper volume of liquid to the reserve,
immediately the first diffusion is finished this saine volume of liquid is taken from the
second diffuser the strength of which has been established with a difference absolutely
the same as that which should exist between the strength of the macerator at the
end of the maceration and the first diffuser at the beginning of the operation. This
addition reestablishes by compensation the normal alkalimetric strength.
The total expenditure of alkalino-caustic salts can be easily calculated. It consists
of the difference between the initial alkalimetric strength of the macerating bath and
that of the same bath after maceration; and the final loss decided upon and fixed
before-hand.
The diffusions having been finished the material under treatment is transferred
without being washed and after simple draining into an agitating vessel in which it
receives a hot treatment with clear water. This boiling, repeated if necessary, has
for object to remove from it matters in combination or not combined and alkalino-
caustic salts which it has carried from the last diffuser. The duration of the boiling
varies from 1 to 2 hours according to the material treated.
It will be understood that there can be nothing absolute in these indications of
duration as the diversity of the materials and the nature of the water necessarily
make it variable; but the termination of these operations is easily ascertained by.
taking a small part of the boiled material and rinsing it in clear water. The appearance
of the fibre, its whity-brown color and the facility with which it separates on being
rubbed by hand are indications that cannot mislead.
The boiling having been finished nothing further is required, if it is wished to
employ the raw fibre, than to thoroughly wash it. If on the contrary it is desired to
bleach it any ordinary bleaching operations can be followed.
The lye residues can be utilized by saponifying them, the operation is easy as the

page_text: residues are eminently fitted therefor. With this object the liquids after having been
allowed to settle are decanted; the magmas, compounds of the alkalino-caustic
matters arising from the combinations during the masceration are deposited at the
bottom of the vessel and are collected to be saponified or sold to soap makers.
There is nothing more, as residues to be rejected than the waters from the boiling
operation the discharge of which into streams might be objectionable. They should
therefore be clarified. They are defecated by treatment with a slight excess of ordinary
hydrochloric acid of commerce. The organic matters precipitate and the waters can
then be run off into streams. The organic precipitates collected have a value as they
can be utilized in the manufacture of manure.
Having now particularly described and ascertained the nature of my said inven-
tion, and in what manner the same is to be performed, I declare that what I
claim is :-
:-
The process hereinbefore described of treating vegetable materials to fit them for
the manufacture of paper, pasteboard, threads, tow or other like objects which process
consists in first submitting the vegetable materials to alkalino-caustic lixiviation, by
maceration, in the open air; secondly to successive diffusions in the open air in alkalino-
caustic liquids the strengths of which are chemically regulated and which become
successively enriched in the humid way by the excess of the alkalino-caustic agent,
of a higher strength, absorbed or taken up in the course of the maceration by the
vegetable material; and thirdly to boiling; the alkalino-caustic liquid employed in
the maceration, a part of which has entered into alkalino-organic combinations or
been taken up by absorption, being reconstituted by the transfer into the macerating
bath of the necessary volume of liquid taken from the first diffusion vessel and by
the addition of a regulated quantity of alkalino-caustic liquid from a reserve supply,
while the strengths and volumes of the series of diffusion vessels are reconstituted by
means of liquids systematically transferred from one diffusion vessel to another, all
substantially as hereinbefore set forth the alkalino-caustic and organic matters con-
tained in the lye residues and in the waters from the boiling operation being sub-
sequently separated if desired, as described.
J. C. MEWBURN,
169, Fleet Street, London,
Agent.