A NEW OR IMPROVED METHOD OF OBTAINING SACCHARINE SUBSTANCES FROM CEREAL AND VEGETABLE MATTERS, AND APPLYING THE PRODUCTS OBTAINED TO VARIOUS USEFUL PURPOSES
Year: 1858

page_text: LETTERS PATENT to Jean Baptiste Adolphe Lombard and Xavier Tristan
Esquiron, both of Paris, in the Empire of France, for the Invention of
"A NEW OR IMPROVED METHOD OF OBTAINING SACCHARINE SUBSTANCES FROM
CEREAL AND VEGETABLE MATTERS, AND APPLYING THE PRODUCTS OBTAINED TO
VARIOUS USEFUL PURPOSES,"
Sealed the 25th November 1858, and dated the 7th June 1858.
PROVISIONAL SPECIFICATION left by the said Jean Baptiste Adolphe
Lombard and Xavier Tristan Esquirou at the Office of the Commis-
sioners of Patents, with their Petition, on the 7th June 1858.
We, JEAN BAPTISTE ADOLPHE LOMBARD and XAVIER TRISTAN ESQUIRON,
both of Paris, in the Empire of France, do hereby declare the nature of the
said Invention for "A NEW OR IMPROVED METHOD OF OBTAINING SACCHARINE
SUBSTANCES FROM CEREAL AND VEGETABLE MATTERS, AND APPLYING THE PRODUCTS
OBTAINED TO VARIOUS USEFUL PURPOSES," to be as follows:-
Our Invention relates, first, to a new mode of effecting the graduated or
progressive saccharification of all cereals, such as barley, wheat, rye, oats,
maize, rice, &c., and of all vegetable matters, such as ligneous fibres, paren-
chyma, pulps, roots, the rind of fruits, the fecula of potatoes, and all feculous
fruits in general, by means of the simultaneous use of water, weakly acidulated
or not, and of apparatus having closed boilers, leated either by a current of
superheated steam, or by an open fire, or by the introduction into these
apparatus of air or any other gaseous body compressed, which delays the

page_text: arrival at the boiling point, the effect of which is, the capability of raising the
temperature of the mixture contained in the apparatus, which we effect either
by a bath of fatty bodies, metal in fusion, or other substances capable of
developing pressure in these apparatus, and consequently heat above two
hundred and twelve degrees Fahrenheit.
Secondly, to the application of all kinds of mineral or vegetable acids, and
by preference, oxalic, sulphuric, & hydrochloric acids, &c. The effect of this
application is to avoid the use of too high a temperature, otherwise a com-
mencement of caramelisation of part of the saccharine matter would perhaps
have to be feared.
Thirdly, to the application of the product obtained (wort) to the
manufacture of all kinds of beer or beverages.
Fourthly, to the application of these processes to the manufacture of syrups,
and to the application of these latter to the distillation and manufacture of
vinegars.
The manufacture of beer and syrups being of vast importance, we have
considered the possibility of substituting a better method for that adopted in
the ordinary manufacture, which we have tried by means the most various.
The methods heretofore know can be reduced (as regards beer) to producing
by the germination of cereals (particularly of barley, by reason of the lowness
of its price and it being casier to treat in order to extract the saccharine
matter,) a particular principle, which is termed "diastasis," which, in the
presence of water, and a temperature of from one hundred and fifty-eight to
one hundred and seventy-six degrees Fahrenheit, acts on the remainder of the
I constituent parts of the seed and transforms them into dextrine and sugar,
which two latter substances, with the addition of hops, are exposed to alcoholic
fermentation. This method has the following serious defects:-The germina-
tion for the preparation of malt is very expensive, in consequence of the area
employed for the germination of the seed being necessarily very large, as it is
only effected in thin layers; the drying of the malt requires great care, and
also entails great expense.
The production of sugar and dextrine by these methods always depends on
the quality of the cereals and on the care taken in the varicus operations
which they undergo, consequently the strength of the beer is very variable,
and can never be predetermined, although produced by the same quantity
of grain.
The drawing of the malt or mashing is done by the arm; this operation
is not only very expensive by reason of the hand labour it requires, but is also
very laborious for the workman.

page_text: The decoction of the hops, especially as effected in most manufactories in
France, where the hops are thrown into the boiler, in which it is combined
with water, and then left to itself, is a very long and imperfect operation.
It is clear that by this method the little essential oil contained in the hops
evaporates, and there only remains in the wort the bitter principles, which
renders the beer very inferior because it is deprived of the perfume sought
for, and moreover will not keep any length of time because the preserving
property is climinated.
The cooling of the beer should be effected very rapidly, otherwise it is
exposed to various alterations which are injurious to its preservation, in
particular, the alterable principles contained in barley consist chiefly of
azoted matters which engender or develop yeast.
Notwithstanding all the treatments which cereals are made to undergo, it is
impossible to utilize all the useful products they contain, and the grains or
residue still contains considerable proportions of starch, which are lost. (As
regards syrups :) It is necessary to use very large quantities of sulphuric
acid, saturation of which afterwards being difficult to obtain, which is a very
serious defect, united to that of the formation of calcareous compounds, which
are injurious to the fermentation, and may sensibly change the taste and
wholesomeness of these products. Being convinced of these objections or
defects, we have discovered how to obviate them by taking advantage of the
property possessed by starch of being completely soluble in water at a tem-
perature above two hundred and seventy degrees Fahrenheit in a closed
Under the influence of
apparatus, preventing the evaporation of the water.
this prolonged action the starch is transformed into dextrine and sugar, in
proportions varying according to the length of the action, which is obtained
by heating the hydrated starch in any apparatus or closed boiler capable of
resisting pressures corresponding to these temperatures. In the numerous
experiments we have made, we have discovered that a slight caramelisation is
produced at the limit of the temperature indicated above; in order to avoid
it we have introduced a minimum proportion of acid, which allows the saino
result to be obtained at a lower temperature without any caramelisation. By
operating thus in the product, more or less concentrated, that is obtained,
there are no azoted matters coagulated and precipitated, as they are by this
high temperature. This completely does away with the operation of the
cooking of the wort with the hops, which operation is indispensable in the
method of manufacture heretofore adopted, which was intended to coagulate
and precipitate these matters by boiling, and also the tannin of the hops.
This latter may then be added in the form of extract (essential oil and solid

page_text: the
matter or bitter principle), which gives great economy in its' use, as there
is no loss of essential oil, which loss is produced by boiling, and besides
economy, a superior quality of product is obtained. It also follows from
the application of these processes that the cooling may be effected without
fear and more slowly, and this by reason of the absence of azoted matters.
The most important point is, that by these means all the useful principles
contained in the cereals are taken advantage of, and the residue consists of
the cortical part o
TREATMENT OF THE MATTERS IN THE CLOSED BOILER.
The mode of operating is very simple for the manufacture of beer. Cereals,
corn, barley, oats, rye, maize, rice, buckwheat, &c., fecula, feculous fruit, and
all substances coutaining starch, must first be reduced to flour or coarsely
ground; it is unnecessary to separate the bran, except in cases when it is
desired to have less residue; tlicy are then sifted in order to have only the
flour to treat. They are mixed some hours before use in once, twice, three,
four, five, six times and more their weight of water; the proportion of water
varies according to the concentration of the products desired to be obtained;
this previous maceration is not absolutely necessary, it may be dispeused with
and the operation may be direct. In this maceration the starch swells, and
consequently has less cohesion and is much more rapidly transformed. This
mixture is then placed in a close boiler or apparatus, furnished with its safety
valve and high-pressure guage. The proportion of acid is then added, which
we cannot fix herein, inasmuch as it varies according to the nature and quality
of the substance and of the cohesion resulting from the stronger or weaker
aggregation and of the quantity of extraneous matters contained in the
substances to be heated. The apparatus is luted and heated by one of the
methods above mentioned. The pressure and the degree of heat vary, like
the proportions of acid, according to the more or less sweetened product
desired to be obtained and according to the substance employed. When the
saccharification has reached the degree desired, we cease heating and allow it
to cool till there is no more pressure and till the temperature has returned
to two hundred and twelve degrees Fahrenheit. This cooling may be accele-
rated by making a current of cold water pass into the apparatus by means of
tubes or by a worm arranged for that purpose. The liquid obtained is then
drawn off, and the saturation of the acid is immediately proceeded with by
means of lime, baryta, strontian, &c., or carbonates of these bases. If sulphuric
acid is used, when its saturation by carbonate of lime is terminated, we add,
while stirring, a little oxalic acid dissolved in water, which precipitates the

page_text: calcareous salts which might be found in solution, and by this incans perfectly
pure products, exempt from all calcareous compounds, are obtained. The
liquid is then drawn off, and if it is not perfectly clear it is clarified by
albumen, white of eggs, blood, &c., or other known means. For this purpose
the inatter is diluted in the liquid while stirring strongly, the liquid is then
carried for some instants to boiling heat by means of a current of steam, and
afterwards filtered. The liquid being cooled, is diluted with water, if con-
centrated, in order to give it the desired density, according to the quality of
beer to be manufactured, and the extract of hops is added in proportions
according to the nature of the beer desired to be obtained. It is then run
into the fermentation vats under the conditions well known in the manufacture
of beer.
For vegetable matters, ligneous fibres, parenchyma, pulps. roots, rind of
fruits, &c., we proceed in. the same way, always employing a much larger
proportion of acid, and increasing the length of the operation, the action, and
also the temperature; these variations depend exclusively on the nature and
composition of the substances to be heated.
For the manufacture of syrups the operation is the same, the length of the
action only is increased; we stop when the alcohol no longer precipitates
dextrine. The syrups thus obtained are then evaporated in order to bring
them to the desired degree of concentration.
We expressly reserve the power of improving our processes, and we desire
to retain during the term of our l'atent the exclusive privilege of any analogous
method, the object of which is the graduated or progressive saccharification
of all kinds of substances by means of closed apparatus and water, either
acidulated or not; these incans and the combination of all others mentioned
forming the basis of our system and the object of our Invention.
SPECIFICATION in pursuance of the conditions of the Letters l'atent filed
by the said Jean Baptiste Adolphe Lombard and Xavier Tristan
Esquiron in the Great Seal Patent Office on the 4th December 1858.
TO ALL TO WHOM THESE PRESENTS SHALL COME, we, JEAN
BAPTISTE ADOLPHE LOMBARD and XAVIER TRISTAN ESQUIRON, both of Paris,
in the Empire of France, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Seventh day of June, in the year of our Lord
One thousand eight hundred and fifty-eight, in the twenty-first year of Her

page_text: reign, did, for Herself, Her heirs and successors, give and grant unto us, the
said Jean Baptiste Adolphe Lombard and Xavier Tristan Esquiron, Herspecial
licence that we, the said Jean Baptiste Adolphe Lombard aud Xavier Tristan
Esquiron, our executors, administrators, and assigns, or such others as we,
the said Jean Baptiste Adolphe Lombard and Xavier Tristan Esquiron,
our 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 "A NEW OR IMPROVED METHOD OF
OBTAINING SACCHARINE SUBSTANCES FROM CEREAL AND VEGETABLE MATTERS, AND
APPLYING THE PRODUCTS OBTAINED TO VARIOUS USEFUL PURPOSES," upon the con-
dition (amongst others) that we, the said Jean Baptiste Adolphe Lombard
and Xavier Tristan Esquiron, our executors or administrators, by an instru-
ment in writing under our 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 Seal Patent Office within six calendar months next
and immediately after the date of the said Letters Patent.
NOW KNOW YE, that we, the said Jean Baptiste Adolphic Lombard
and Xavier Tristan Esquiron, do hereby declare the nature of our said
Invention, and in what manner the same is to be performed, to be par-
ticularly described and ascertained in and by the following statement, that
is to say:
Our Invention relates, first, to a new node of effecting the graduated or
progressive saccharification of all cereals, such as barley, wheat, rye, oats,
maize, rice, &c., and of all vegetable matters, such as ligneous libres, paren-
chyma, pulps, roots, the rind of fruits, the fecula of potatoes, and all feculous
fruits in general, by means of the simultaneous use of water, weakly acidulated
or not, or of the different substances further described, and of apparatus
having closed boilers heated either by a current of superheated steam or by
an open fire, or by the introduction into these apparatus of air or any other
gaseous body compressed, which delays the boiling point, the effect of which
is the capability of raising the temperature of the mixture contained in the
apparatus, which we effect either by a bath of fatty bodies, metal in fusion
or other substances capable of developing pressure in these apparatus, and
consequently heat above 212° Fahrenheit.
Secondly, to the application of all kinds of mineral, of vegetable acids, and
by preference oxalic, tartric, sulphuric, & hydrochloric acids, &c. The object

page_text: of this application is to avoid the use of too high a temperature, otherwise
a commencement of caramelisation of part of the saccharine matter would
perhaps have to be feared, alterations which are to be feared by the great
inconveniences it presents in certain manufactures.
Thirdly, in introducing in these apparatus or boilers all liquid or gaseous
bodies, and by preference carbonic acid, for manufacturing beers, beverages,
or sirups; the chlorine gas, or a dissolution of hypochlorite for manufacturing
alcohol without using acid, chlorine, or hypochlorite; the degree of solubility
of the starch which is contained in the cereals or other feculous matters, in
the treatment by water, heat, and pressure, is too elevated, and caramelisation
would be unavoidable.
It is then very important not to surpass a certain number of degrees,
339 degrees Fahrenheit, maximum, and to operate at a lower degree if possible.
But as the pressure corresponding to these temperature is not sufficient, it is
necessary, with a compression pump or by any other similar means, to conduct
in the boiler a current of free or compressed gas, according to the conditions
in which the operation is conducted; this current determines an overcharge
of pressure, the effect of which is to accelerate the solubility, the combination,
and the hydrating of the starch, in effect similar to that of the acid, of which the
advantage is to operate at a lower temperature to that of the caramélisation.
For such substances as parenchyma, ligneous cellular fibres, &c., it is operated
by similar means above mentioned, in conditions varying according to the
nature of the matter and its greater or less agregation.
Fourthly, in applying obtained products (wort) to the manufacture of all
kinds of beers or beverages.
Fifthly, in applying these processes to the manufacture of sirups, and the
application of the last to the manufacture of alcohols and vinegars.
The manufacture of beer and sirups being of vast importance, we have
considered the possibility of substituting a better method for that adopted in
the ordinary manufacture, which we have tried by means the most various
The methods heretofore known can be reduced (as regards beer) to producing
by the germination of cereals (particularly of barley, by reason of the lowness
of its price and it being easier to treat in order to extract the saccharine
matter,) a particular principle which is termed "diastasis," which, in the
presence of water, and a temperature of from 158° to 170 Fahrenheit, acts
on the remainder of the constituent parts of the seed, and transforms them
into dextrine and sugar, which two latter substances, with the addition of
hops, are exposed to alcoholic fermentation. This method has the following
serious defects:-

page_text: The germination for the preparation of malt is very expensive in con-
sequence of the area employed, for the germination of the grain being
necessarily very large, as it is only effected in thin layers; the drying of
the malt requires great care and also entails great expense.
The production of sugar and dextrine by these methods always depends on
the quality of the cercals and on the care taken in the various operations which
they undergo, consequently the strength of the beer is very variable, and can
never be predeterminated although produced by the same quantity of grain.
The drawing of the malt or mashing is done by the arm; this operation
is not only very expensive by reason of the hand labour it requires, but is
also very laborious for the workmen.
The decoction of the hops, especially as effected in most manufacturies in
France, where the hops are thrown into the boiler in which they are
combined with water and then left to themselves, is a very long and imperfect
operation; it is clear that by this method the little essential oil contained in
the hops evaporates, and there only remains in the wort the bitter principles,
which renders the beer very inferior because it is deprived of the perfume
sought for, & moreover will not keep any length of time because the
preserving property is eliminatod.
The cooling of the beer should be effected very rapidly, otherwise it is
-exposed to various alterations which are injurious to its preservation; in
particular, the alterable principles contained in barley consist chiefly of
azoted matters which engender or develop yeast.
Notwithstanding all the treatments which cereals are made to undergo, it
is impossible to utilize all the useful products they contain, and the grains or
residue still contain considerable proportions of starch, which are lost. (As
regards syrups :) it has been necessary heretofore to use very large quantities
of sulphuric acid, the saturation of which afterwards being difficult to obtain,
which is a very serious defect, united to that of the formation of calcarious
compounds, which are injurious to the fermentation, and may sensibly
change the taste and wholesomeness of these products.
Being convinced of these objections or defects, we liave discovered how to
obviate them by taking advantage of the property possessed by starch of being
completely soluble in water at a temperature above 212° Fahrenheit, but
which must never exceed 370° Fahrenheit, in a closed apparatus, preventing the
evaporation of the water. Under the influence of this prolonged action, the
starch istransformed intodextrine andsugar, inproportions varying according to
thelength of the action, which is obtained by heating the hydrated starch indry
apparatus or closed boiler,capable of resisting pressures corresponding to these

page_text: temperatures. In the numerous experiments we have made, we have dis-
covered that a slight caramelisation is produced at the limit of the tempera-
ture indicated above; in order to avoid it we have introduced a minimum
proportion of an acid or of a gas, which allows then the same result to be
obtained at a lower temperature without any caramelisation; by operating thus
in the product or less concentrated that is obtained, there are no azoted
matters coagulated and precipitated as they are by the higher temperature ;
this completely does away with the operation of cooking or treating of the
wort with the hops, which operation is indispensable in the method of manu-
facture heretofore adopted, which was intended to coagulate and precipitate
these matters by boiling, and also the tannin of hops. This latter may then
be added in the form of an extract (essential oil and solid matter or bitter
principlo), which affords great economy in its use, as there is no loss of
essential oil, which loss is produced by boiling, and besides the economy, a
superior quality of product is obtained.
This addition of hops under the form of extract, is not indispensable, the
worts when obtained may equally be treated by the actual means without
any inconvenience arising. It also follows from the application of these
processes, that the cooling may be effected without fear and more slowly,
and this by reason of the absence of azoted matters; the most important point
is, that by these ineans all the useful principles contained in the cereals are
taken advantage of, and the residue consists of the cortical part ouly.
TREATMENT OF THE MATTERS IN A CLOSED BOILER.
The mode of operating is very simple for the manufacture of beers, alcohols,
cercals (corn, barley, oats, rye, maize, rice, buckwheat, &c.), fecula, feculous
fruits, and all substances containing starch, must first be reduced to flour or
coarsely ground; it is unnecessary to separate the bran, except in cases where
it is desired to have less residue, they are then sifted in order to have only
the flour to treat; they are mixed some hours before use in once, twice, three,
four, five, or six times, and more, their weight of water; the proportion of
water varies according to the concentration of the products desired to be
obtained; this previous maceration is not absolutely necessary, it may be dis-
pensed with and the operation may be direct. In this maceration the starch
swells, and consequently has less cohesion and is much more rapidly trans-
formed; this mixture is then placed in a close boiler or apparatus furnished
with its safety valve & high-pressure guage. If seeds are treated by acid
the proportion of the acid is then added, which we cannot fix herein, inasmuch

page_text: as it varies according to the nature and quality of the substance, and of the
cohesion resulting from the stronger or weaker agregation and of the quantity
of extraneous matters contained in the substances to be treated. The appa-
ratus is Inted and heated by one of the methods above mentioned. The
pressure and the degree of heat vary, like the proportions of acid, according.
to the more or less sweetened product desired to be obtained, and according
to the substance employed.
When the saccharification has reached the degree desired, we cease
heating, and allow it to cool till there is no more pressure, and till the tem-
perature has returned to 212° Fahrenheit; this cooling may be accelerated
by making a current of cold water pass into the apparatus by means of tubes,
or by a worm arranged for that purpose. The liquid obtained is then drawn
off & the saturation of the acid is immediately proceeded with by means of
lime, baryta, strontian, &c., or carbonates of these bases. If sulphuric acid is
used, when its saturation by carbonate of lime is terminated, we add, while.
stirring, a little oxalic acid, or an oxalate of ammonia dissolved in water, which
precipitates the calcareous salts which might be found in solution,and by this
means perfectly pure products, exempt from all calcareous compounds, are.
obtained. The liquid is then drawn off, and if it is not perfectly clear it is
clarified by albumen, white of eggs, blood, &c., or other known means. For
this purpose the matter is diluted in the liquid while stirring strongly; the
liquid. is then carried for some instants to boiling heat by means of a current.
of steam and afterwards filtered. The liquid being cooled is diluted with
water, if concentrated, in order to give it the desired density, according to
the quality of beer to be manufactured, and the extract of hops is added in
proportions, according to the nature of the beer desired to be obtained; it
is then run into the fermentation vats, under the conditions well known in
the manufacture of beer.
For vegetable matters, ligneous fibres, parenchyma, pulps, roots, rind of
fruits, &c., we proceed in the same way, always employing a much larger
proportion of acid, and increasing the length of the operation, 'the action,
and also the temperature; these variations depend exclusively on the
nature and composition of the substances to be treated.
For the manufacture of syrups the operation is the same, the length of
the action only is increased, we stop when the alcohol no longer precipitates
dextrine; the syrups thus obtained are then evaporated, in order to bring
them to the desired degree of concentration.
We have represented in the annexed' Drawing, as a specimen, one of the

page_text: ratus.
apparatus weemploy for the saccharification of cereals at high or low pressure;
in giving a drawing of this apparatus, we do not confine ourselves to the forms
and dispositions indicated, which may vary according to the nature of the
substances to be treated, of the product to be obtained,and of the means to be
employed. The Drawings show an elevation, partly in section, of the appa-
u, furnace; b, boiler and its accessories; c, feeding apparatus;
d, worm, communicating by both extremities with the boiler b; c, recipient.
containing the seed or feculous matter, and the water, acidulated or not;
the whole is heated by the worm d to the temperature and to the pressure
required; the tubes communicating from the boiler to the worm are provided
with cocks;, emptying cock; y, syphon or gauge; h, valve; i, pyrometer or
thermometer at high temperature; j, manometer or pressure gauge; k, suction
pump, for the introduction into boiler e of a neutral gas, for instance, carbonic
acid, which serves to establish the pressure; l, recipient provided with a
manometer; m, tube, conducting the carbonic acid from the recipient / to
the boiler e; this tube is provided with cocks; n, tube, causing the pump to
communicate with a generator of carbonic acid gas.
The apparatus works in the following manner :-The grain or feculous
matter, the water pure or not, are thrown in the recipient e; the boiler bis
heated, and by a current of steam it elevates the mixture (contained in the
said recipient)to a temperature corresponding to 4 atmospheres, for instance,
temperature at which caramelisation is not to be feared.
At this moment,
and by means of a compressing apparatus l, a current of carbonic acid gas, for
instance, is injected in the boiler or recipient e; the effect of this is to
determine an overcharge of cold pressure, varying according to the nature of
the product to be treated under the influence of the water, of the heat, of the
acid or not, of a current of gas or not, according to the mode of operating.
The matter treated is completely saccharified in a length of time which
cannot be determined here, because it varies according to each quality of
grain, &c.
The saccharification once obtained with the desired proportions of dextrine
and of sugar, the liquid is drawn off and is treated by the known means of
fermentation and of manufacturing.]
We expressly reserve the power of improving our processes, and we desire to
retain during the term of our Patent the exclusive privilege of any analogous
method,theobject of whichisthe graduated or progressive saccharification of all
kinds of substances, by means of closed apparatus and water,either acidulated
or not; these means, and the combination of all others mentioned, forming the

page_text: basis of our system and the object of our Invention. This saccharification
may vary in time from 45 minutes to 10 hours, according to the greater
or less aggregation of the matters to be treated and the mode of treating
either; the operation takes place with or without acid.
In witness whereof, we, the said Jean Baptiste Adolphe Lombard, and
Xavier Tristan Esquiron, have hereunto set our hands and seals, this
Thirtieth day of November, in the year of our Lord 1858.
J. B. ADOLPHE LOMBARD.
T. ESQUIRON.
(L.S.)
(L.S.)