IMPROVEMENTS IN THE PREPARATION OF VEGETABLE MATTERS AS A PULP FOR THE MANUFACTURE OF PAPER
Year: 1860

page_text: LETTERS PATENT to Julien Denis, of Queenhithe, in the City of London,
Merchant, for the Invention of "IMPROVEMENTS IN THE PREPARATION OF
VEGETABLE MATTERS AS A PULP FOR THE MANUFACTURE OF PAPER."—A com-
munication from abroad by Mr. Henry Bouchet, of Quai Montebello,
Paris, in the Empire of France.
PROVISIONAL SPECIFICATION left by the said Julien Denis at the
Office of the Commissioners of Patents, with his Petition, on the
15th May 1860.
I, JULIEN DENIS, of Queenhithe, in the City of London, Merchant, do
hereby declare the nature of the said Invention for "IMPROVEMENTS IN THE
PREPARATION OF VEGETABLE MATTERS AS A PULP FOR THE MANUFACTURE OF PAPER,"
to be as follows:-
My improved method of converting textile plants into a pulp is as follows:-
I put into a wooden or metal tub a ton, or a ton and a half of raw material.
For every 2 cwt. of raw material I dissolve 22 lbs. of sub-carbonate of soda in
22 gallons of hot water; when the dissolution is perfect, I throw in 5 lbs. of
liquid chlorine drawn clear, marking one degree of the acidimeter Beaumé.
1 add this proportion to the materials already in the tub. It is necessary that
the lye should be 5 or 6 inches from the top of the materials, as the steam
which condenses in the tub often produces too much water. The tub must be
furnished with a lid or cover, which is shut down to keep in the steam; the
mass is to be boiled for 6, 8, 10, or or sometines 12 hours, according as the
materials are more or less difficult to reduce.
2ndly, when the materials are well boiled I put them into a reducing
cylinder, which reduces them to fibre of two or three inches in length, washing

page_text: it at same time by the introduction of pure water entering through a suitable
cock, which water is carried off by another cock; for this operation 2 or 3
hours suffices. The materials are then taken from the cylinder and put into a
receptacle ready for further treatment.
3rdly, textile plants usually contain sulphate of iron or copper, which, as
Jong as they exist in the plants, render the bleaching not only very difficult,
but very costly, besides weakening the fibre. I proceed in this operation to
neutralize the sulphate of iron as follows:-I make a bath of muriatic acid
marking one degree of the acidimeter Beaumé, and then add to this bath
about one pound of marine salt to every 22 gallons of water. I work this up
well, and throw into it the materials out of the tub. It is necessary that the
materials in the bath should not be too thick, so that a man can work it well
so as to separate it in the bath; three hours steeping in this bath is sufficient,
after which the liquid is to be withdrawn and used again, as will be explained
hereafter. After this the pulp should be washed in the tub with 3 waters; it
is then taken out and put into suitable receptacles to drain, from thence to
undergo the next operation. To neutralize the sulphate of copper I make a
bath of sulphuric acid marking one degree of the acidimeter of Beaumé, & add
to it in equal quantities marine salt, salts of nitre, or uitrate of soda, and
proceed as above mentioned. I have before mentioned that this bath should
be reserved, because it may be used again by adding to it half the ingredients
above named, and a sufficient quantity of pure water. These baths may be
slightly heated without injury to the materials.
4thly, I make a bath of liquid chlorine marking one degree of the acidimeter
Beaumé to well saturate two cwt. of material which have been placed in the
bath of acid, amounting to 154 or 176 gallons; I dissolve in it 5 lbs. of sub-
carbonate of soda, or sulphuret of soda, nitrates, phosphates, azotates, silicates,
aluminas, carbonate of lime, or any chemical products which are soluble and
contain carbonic acid or azote, and which have also some power of decolo-
rization, which I add to the chlorine to netralize its acidity, for as soon as the
substances are dissolved, the bath becomes of an unctuous nature. I can heat
this bath to a temperature of 20 to 25 degrees centigrade, or even to 50 or 60
degrees without injury to the materials, although it is well known by all paper
manufacturers that they could not hitherto heat their chlorine even to ten
degrees without burning the materials submitted to its action. When the bath
is heated to the above temperature, I put into it the material, which I leave
for 3 or 4 hours, taking care to well stir it every half hour. This operation
ended, I reserve this bath for after uses, as I will explain. I now wash the
material in the tub and take it out to drain.

page_text: 5thly, I make a bath of chlorine marking two degrees of the acidimeter
Beaumé, and for this bath I prefer to any other the nitrate of soda, and
always in the proportion of 5 lbs. to every 154 to 176 gallons; I heat this
bath to 15 degrees centigrade, and proceed as in the fourth operation. I
preserve this bath in a separate reservoir, and use it subsequently for the
fourth operation, by adding to it half the amount of ingredients & chlorine
employed to make the former bath.
6thly, and last operation, after the bath No. 5 I wash the pulp, and if it is
to be of a superior whiteness, I throw into the bath 6 or 8 gallons of
chlorine at two degrees, shutting off for half an hour the influx and efflux of
After this I bathe it with a great quantity of water, and before taking
the pulp out I throw into it (dissolved in water) from an ounce and an half to
two ounces of proto-chloride of tin, to disinfect the pulp and neutralize tho
acids, as well as to prevent the pulp or the paper subsequently turning yellow.
To keep and distribute this pulp to the manufacturers it must be dried. I
have before stated that the water of No. 4 bath should be preserved, as it is
useful for steeping the raw material, therefore no fresh chlorine is required;
but I always add 22 lbs. of sub-carbonate of soda for every cwt. of material to
be treated.
D..
lothed I am enabled to convert all fibrous plants into a
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Julien Denis in the Great Scal Patent Office on the
15th November 1860.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JULIEN
DENIS, of Queenhithe, in the City of London, Merchant, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Fifteenth day of May, in the year of our Lord
One thousand eight hundred and sixty, in the twenty-third year of Her reign,
did, for Herself, Her beirs and successors, give and grant unto me, the said
Julien Denis, Her special licence that I, the said Julien Denis, my
executors, administrators, and assigns, or such others as 1, the said Julien
Denis, 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 "IMPROVEMENTS IN THE PREPARATION

page_text: OF VEGETABLE MATTERS AS A PULP FOR THE MANUFACTURE OF PAPER," a com-
munication from abroad by Mr. Henry Bouchet, of Quai Montebello, Paris,
in the Empire of France, upon the condition (amongst others) that T. the
said Julien Denis, my executors or administrators, by an instrument in
writing under my, or their, or one of their hands and seals, should par-
ticularly 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 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 Julien Denis, do hereby declare the
nature of the said Invention, and in what manner the same is to be per-
formed, to be particularly described and ascertained in and by the following
statement, reference being had to the Sheet of Drawings hereunto annexed,
and to the letters and figures marked thereon (that is to say) :-
Raw textile plants in an unmanufactured state, unlike rags which are worn
by personal use, and reduced by washing and alkalies, contain more or less of
foreign substances which must be separated from their celular tissue, such as
gum, gluten, resin, oil, iron, tin, sulphur, &c. Henco to compare them with
rags by submitting them to treatment similar to or in combination therewith,
would produce but a negative result, and all the attempts made in that
direction have failed, by reason of the parties so attempting to combine or use
them being unacquainted with the objections to the combination, therefore
ignorant of the proper remedy to be applied. It will be understood that the
first step in this manufacture should be the study of the nature of the textile
plants to be converted into paper pulp, in order to apply to them treatment
suitable to their nature and condition.
The manufacture of paper is so extensive a character that rags are not
alone sufficient to supply the wants of that manufacture, therefore other
materials must be substituted.
This Invention relates to an entirely new treatment of textile plants for
converting them into paper pulp, consisting of,-
1st, a new chemical composition for the steeping, which in its effect destroys
the gums, resins, oils, and fecula without altering the fibre of the plant.
2ndly, the extraction by means of new compositions, of hydrochloride,
sulphuric, and nitric acids, of the sulphates of iron and tin the plants contain.
3rdly, of new combinations of chlorines, which are considerably reduced in
strength, by which means they may be beated without danger to the tenacity
of the fibre to forty degrees centigrade, about one hundred and four degrees
Fahrenheit.

page_text: 4thly, the novel application of a chemical agent to disinfect the matters and
neutralize the acids.
5thly, of a new form of plate as a purifier in the cylinder-pulping engine.
And, lastly, in the method of treatment which insures the production of a
good and fine pulp for paper.
It will be unnecessary in this Specification to ennumerate the names of all
the textile plants which are more or less suitable for the production of paper
pulp, as also to describe their individual peculiarities. However, to render the
description as complete as possible, I will here indicate the plants best suited
for the purpose, and the manner of treating them, which is described in this
Specification. The coarser species are the broom, dwarf and other palms,
diss, formium tenas, wild hemp of America, all kinds of indigenous and exotic
rushes and reeds, the wild flax of Africa, certain barks of trees, such as
mabaut peinant, mahaut vincent, cabbage tree, balasier, Spanish rush or
broom, lime and mulberry trees; and, in the second place, as being easier to
treat, requiring only half or two thirds of the quantity of solution necessary
for the above. Some of the finer kinds are maize, yucca glorissa, yucca
filamentosa, colza, cactus, ananas, climus arénarius, elimus giganteus.
The following operations are numbered, in order that they may be more
readily described and understood, and the directions adhered to by those wishing
to avail themselves of this method of treatment. The chemical indredients
employed to combine with the chlorine and acids are potash of soda, sulphato
of soda, nitrate of soda, carbonate of soda, sulphate of potash, salt of ammonia,
carbonate of ammonia, carbonate of potash, carbonate of lime, silicates.
carbonates, phosphates, sulphates of ammonia, hypochloride of lime, bicar-
bonate of potash, and, lastly of all, chemical products and matters which
contain carbonic acid, carbon, mineral, vegetable, and animal alkalies pos-
sessing bleaching properties applicable to the present Invention.
Composition of a bath of chloride of calcium.-For every two hundred and
twenty-five pounds of pulp I form a bath of chlorine containing about one
hundred and fifty gallons, marking the degree of the acid meter Beaumé herein-
after indicated for each operation. In a separate vessel of warm water is
dissolved about five and a half pounds of one of the ingredients above
mentioned, or equal parts of five or six of these ingredients may be taken to
form the solution. When the matters are dissolved they are poured on to the
bath of chlorine, which is then heated to seventy, eighty, or one hundred
degrees Fahrenheit, according to the requirement of the operation, as will bo
herein-after indicated. The baths are composed of sulphuric and hydrochloric
acids, to which is added about three pounds of nitrate of soda for every one

page_text: hundred and fifty gallons of a certain strength. These baths have for object
to destroy the sulphate of iron aud copper which may be in the plants. Tho
lyes, which I render caustic with lime water, are composed of sub-carbonate
of soda, carbonate of potash, ammoniacal salts, and sulphate of soda. The
acids and chlorides are mixed in the washing and pounding cylinder, which
also disinfects the pulp, and preserves the paper for any length of time. The
pulp is purified in the crushing or pulping cylinder engine by means of a
purifying plate of a new form, herein-after described and represented in the
Drawing, which merely consists of a plate of iron galvanized, or of other
suitable metals having perforations through it, as shown.
MODE OF PROCEEDING FOR CONVERTING TEXTILE PLANTS INTO PULP
FOR PAPER.
1st operation.-Steeping and weight of ingredients for every two hundred
and twenty-five pounds of raw material, such as one of the coarser plants (or
those most difficult to treat) above enumerated. The lye is prepared as
follows: In a vessel of warın water are dissolved about twenty-two pounds of
carbonate of soda, about six and a half pounds of sulphate of soda, about four
and a half pounds of sal animoniac; this solution is poured in a vat suitable to
contain half a ton of the raw material, with about seven gallons of chlorine at
two degrees, in another vessel is dissolved about seventeen and a half pounds
of quick lime in cold water, which is allowed to settle, and is drawn off' when
clear; the two solutions are then thrown into the matters contained in the
steeping vat, which is closed and caused to boil until the plants are well
softened, which generally takes from ten to twelve hours for the bardest
materials. If the two solutions do not afford sufficient liquid for keeping the
material moist the necessary quantity should be added.
2nd operation. The material is taken out of the vat and placed in a
cylinder pulping engine; in this cylinder there is a platform or raising piece,
on which is placed the purifying plate; a proper proportion of the material is
then placed in the pulping engine, which is well stirred about and washed;
the cylinder should not be raised far from the plate, so as to rather crush than
cut the fibres, which are to be reduced to about two or three inches in length,
and after being well washed till the washing liquid comes away quite clear;
the material is then placed in a discharging vat to drain.
3rd operation. In a vat containing from one hundred and fifty to one
hundred and seventy gallons, with a double bottom for draining the matters,
is formed a bath of hydrochloric acid marking two degrees of Beaumé's acid
meter; in this is dissolved about two and a half pounds of nitrate of soda; the

page_text: liquid is then well stirred, the acid becoming changed into nitro-hydrochloric
acid, which is the best for dissolving the iron; this bath may be replaced by a
bath of nitric acid, which operates perhaps more effectually, but which has the
disadvantage of being more expensive. In this mixture is placed about two
hundred and twenty-five pounds of material prepared according to the second
operation, which is allowed to steep from three to four hours; it is to be thrown
in at three or four different times, and each portion stirred well, and also
during the operation. The material is afterwards withdrawn, and the bath
preserved, which, by adding one-fourth of the quantity of ingredients at each
time, will serve from ten to twelve times; the material is then washed in the
different waters, taking care to well drain it each time.
4th operation. The vat employed is similar to the last, except that there is
a steam pipe in connection therewith attached to a junction, and which reaches
to within six inches of the bottom. A bath of about one hundred and fifty
gallons of chloride of calcium is formed therein of one and a half degrees acid
meter Beaumé; next is dissolved in four or five gallons of warm water about
six and a half pounds of sub-carbonate of soda, or any other of the above-
mentioned ingredients; this solution is then thrown into the bath, and the
whole well stirred and heated to form from seventy to ninety degrees Fahren-
heit;
the pipe is then removed, and about two hundred and twenty-five pounds
of material of the third operation added; this is allowed to remain about
four hours, being stirred up every half hour. After the material is withdrawn
from the vat preserve the bath, which will form a solution for the stoeping
instead of pure water; the matter is then well washed as before when leaving
the bath of acid, and allowed to drain.
5th operation. The vat made use of is similar to the last, in which a bath
of acid is formed marking two degrees of the acid meter Beaumé ; about six
pounds of nitrate of soda is then dissolved in warm water, and the solution
poured into the bath, which is heated to about seventy degrees Fahrenheit;
the steam pipe is then withdrawn, and about two hundred and twenty-five
pounds of material resulting from the fourth operation added, which is allowed
to steep from five to six hours, stirring five or six times. After this time the
solution is then drawn off, which may be used again for the fourth operation,
with the addition of about twenty-two gallons of chlorine at two degrees, and
about three and a half pounds of subcarbonate of soda. This pulp is then
washed in the vat, as in the two preceeding operations, which will form a white
pulp suitable for newspapers.
6th operation. The pulp of the fifth operation is passed into a washing
engine furnished with a drum washer, and washed for twenty minutes, and if

page_text: it is to be washed to produce a still whiter pulp, the inlet and outlet of the
water are closed, and about ten or twelve gallons of chloride of calcium at two
degrees thrown in, and continue the operation twenty-five minutes longer;
after this put into a vessel containing three or four gallons of pure water about
three and a half pints of sulphuric acid, in which is dissolved about three and
a half ounces of nitrate of soda, and the whole distributed equally over the
material, which is again agitated for ten minutes, and after which open the
entrance and exit of the water, and allow the washing to proceed for half an
hour; the ingress and egress of the water are then shut, and the mixture of
nine quarts of water with about three and a half ounces of proto-chloride of
tin added, which is agitated for ten minutes, and then washed for a quarter of
an hour, for the purpose of decomposing the acid and disinfecting the pulp.
Having described the nature of the Invention, and the manner of per-
forming the same, I declare that what I claim as the Invention of improve-
ments in the preparation of vegetable matters as a pulp for the manufacture
of paper, to be protected by the herein-before in part recited Letters
Patent is,
First, the use and application of the chemical composition herein-before
described for steeping the textile plants.
Secondly, the application of baths of chlorine combined with carbonated
agents, containing, among others, carbonic acid, and which are used in a
heated state.
Thirdly, the application to textile plants of hydrochloric and sulphuric acid
baths, combined or not with nitrate of soda.
Fourthly, the application of proto-chloride of tin for neutralizing the acids
and disinfecting the pulp.
Fifthly, the form of purifier herein-before described and represented.
And, lastly, I claim generally the method of procceding in converting textile
plants into white or brown pulp for paper, herein-before described.
In witness whereof, I, the said Julien Denis, have hereunto set my
hand and seal, this Fifteenth day of November, in the year of our
Lord One thousand eight hundred and sixty.