Improvements in or relating to the Manufacture of Maltose or to the Fermentation of Amylaceous Matter.
Year: 1889

page_text: Date of Application, 1st Apr., 1889
· Complete Specification Left, 19th Sept., 1889-Accepted, 21st Dec., 1889
f
PROVISIONAL SPECIFICATION.
Improvements in or relating to the Manufacture of Maltose or to
the Fermentation of Amylaceous Matter.
A communication from abroad by LA SOCIÉTÉ GÉNÉRALE DE MALTOSE, of Brussels,
in the Kingdom of Belgium, Manufacturers of Maltose.
I, WILLIAM PHILLIPS THOMPSON F.C.S., M.I.M.E., of the Agency for Foreign
Patent Solicitors, 6 Lord Street, Liverpool, and 6 Bank Street, Manchester, both in
the County of Lancaster, and 323 High Holborn in the County of Middlesex, Civil
Engineer, do hereby declare the nature of this invention to be as follows:-
This process being based on new data, it is necessary to make some preliminary
remarks in order to make clear the description that follows.
It has been proved that the amount of diastase which germinating grains contain
does not generally correspond in practice with the nominal amount which should be
produced; theoretically a minimum quantity of malt should by its yield of active
matters convert into saccharine a considerable quantity of amylaceous matter.
:
It is found on the contrary. in practice that a relatively considerable quantity of
malt must be used to arrive at even an imperfect degree of saccharification.
The cause of this phenomenon is found to be in an impairing of the diastase
through the development of ferments which are harmful to it. Thus it is that malt
worts left at the usual temperature for saccharification become gradually weaker and
at the end of a longer or shorter but always relatively short time, lose all their
activity..
$
The same phenomenon appears during the period of saccharification of amylaccous
matters by malt; the germs of the ferments, so abundant in germinating grains
are developed little by little in worts and gradually arrest the action of the
diastase.
To remedy this difficulty, it has been proposed to add to worts undergoing
Saccharification various acids, such as nitric, hydrochloric or sulphuric. These acids
preserve the worts more or less from alteration. Unfortunately, the quantities of
these acids necessary to give this result weaken the diastase to a very considerable
degree and the final result is that nothing or very little, as regards saccharification, is
gained by their use.
.
The present mode of preserving the worts undergoing saccharification generally
consist of assisting them by means of the temperature and by chemical agents not
favourable to the development of harmful ferments. But still the desired result has
not been attained, for on the one hand, simple infusions of malt are mixed with the
worts, which always contain ferments and on the other hand the chemicals being
placed in a diluted material cannot act efficaciously and thus preserve the diastase
intact..
.
Taking these facts into consideration it has been tried to purify malt by an
antiseptic which in weak doses should have no action on the diastase, while at the
same time it should destroy the germs of other ferments.
In their researches my correspondents have discovered that hydrofluoric acid will
attain this result.
In fact by adding to a litre of infusion of malt corresponding to about 200 to
300 grammes of malt, two or three drops of commercial hydrofluoric acid, they can
preserve it for 8 to 10 days without the liquid undergoing the least alteration or
losing any of its saccharifying principle.
My correspondents have besides discovered that an infusion of malt acidulated by
hydrofluoric acid in the above named proportions has its maximum saccharifying

page_text: power at 25-30° C. and not at the temperature of 50-60° C. usually employed for
this purpose.
The preliminary purification of the malt by hydrofluoric acid allowed them to
obtain a very economical working by which means a very considerable saccharification
was realized from a small quantity of malt.
Further, their first successes led them to apply the same principle to the fermen-
tation and their experiments have shown that hydrofluoric acid has a very favourable
action on the yeast, that it prevents the development of other ferments and that its
employment increases by this means very considerably the yield of alcohol.
J. Preparation of infusion of malt and diastase in the form of a concentrated
extract.
There is added to crushed malt diluted with two or three times its volume of cold
water; 10 to 20 grames of commercial hydrofluoric acid-(containing, about 23% of
pure hydrofluoric acid) for every hundred litres of the liquid, taking care.to.keep the
malt in suspension for some time.
This operation deprives the malt of every germ of foreign, fermonts and at the same
time produces a liquid quite suitable for employment as a liquefying and saccharify-
ing agent. According to the amount of work which this liquor.must perform, at the
ond of some hours the hydrofluoric acid is neutralized by means of carbonate.of..lime
or left as free acid when the liquor must produce saccharification, in materials already
containing lime salts.
.
Instead of employing as already shewn the diastasic liquor, the dregs can also first
be separated, so as only to preserve the amylin and the extract. This amylin and
extract can be used as they are, or can be still further separated. by filtration or.by
decanting or by turbinage and a clear or almost clear liquid is then obtained which
forms an unchangeable infusion. By evaporating this liquid in a vacuum at a
maximum temperature of 65-70° C. solid diastase is produced in the form of a
yellowish powder an equal weight of which possesses a saccharifying, action 25 to
30 times stronger than that of malt. The temperature of 65° C. must not be exceeded
when a product is to be obtained of a highly saccharifying power..
II. Manufacture of liquid syrups and of crystals.
As raw material maize.is employed. by preference, although this mode of working
is adapted equally to starch and all. other amylaceous materials. To maize steeped or
unsteeped, ground or unground is added three or four times its volume of water and
it is then boiled under a pressure of three or four atmospheres for one or two hours
by means of the usual apparatus. The boiling being finished the liquid. is cooled to
30 or 40° C. either by addition of cold water or by means of a refrigeratore at the
surface or by any other mode... When brought to this temperature the diluted malt,
or the infusion with amylin or the .clear extract of inalt or even the solid diastase
prepared as detailed in the preceding paragraph I. is added thereto;
The temperature of the liquid.after the addition thereto of the infusion should fall
to 15-25° C. and.it is then left for saccharification of which the duration may vary
from several hours to 48 hours.according to the nature of the product it is wished, to
obtain and the quantity of dextrine it is wished to retain therein.
1
If the materials.contain dregs,in suspension as is the case with maize and cereals.
generally, after two or three hours.they can be separated, either by means of a filter
press or by turbinage or by sifting, or by any other method generally employed. The
filtered liquor is then passed into the settling vats where the saccharification goes on
vigorously at a temperature of about 20° (."
According to whether it is wished to obtain a syrupy or solidified product, the
saccharification is arrested more.or.less quickly; the liquor is then boiled with a little
carbonate of limo: Afterwards. the liquor is evaporated, at 38. to. 42° Beaumé after a
preliminary filtration on any kind of filter.
III: Alcoholic fermentation..
My correspondents system of making alcohol.is based on the same method as that
for the manufacture of syrups as shewn above.

page_text: Maize, or other similar articles, with or without previous bruising must be
thoroughly crushed under pressure.
Diastase, with the addition of hydrofluoric acid as described above, is then added in
one of the forms and at the temperature named for the manufacture of syrups, either
in the form of concentrated diastase or in the form of a clear infusion with or without
amylin or finally in the form of ground malt.
As soon as the saccharification is thoroughly commenced yeast is added to the
liquid; filtered, or not, which has remained for several hours in contact with hydro-
fluoric acid used at the rate of 15 to 20 gr. of acid of commerce (at about 20 %.of
pureracid) per hectolitre of liquid yeast.
The employment of a diastasic agent and of a yeast, very active and deprived of
the elements in them detrimental to alcoholic fermentation, allows of obtaining
regularly a return of 38 litres of alcohol per 100 kilos. of maize containing 63% of
amyliu.
Datildi. 20th day of Murah 1980
WM. P. THOMPSON & Co., ·
Agents for the Applicant.
COMPLETE SPECIFICATION.
Improvements, in or relating to the Manufacture of Maltose or to
the, Fermentation of Amylaceous Matter.
A communication from abroad by LA SOCIÉTÉ GÉNÉRALE DE MALTOSE, of Brussels,
in the Kingdom of Belgium.
1, WILLIAM PHILLIPS THOMPSON, F.C.S., M.I.M.E., of the Agency for Foreign
Patent Solicitors, 6, Lord Street, Liverpool and 6, Bank Street, Manchester, both in
the County of Lancaster, and 323 High Holborn, in the County of Middlesex, Civil
Engineer, do hereby declare the nature of this invention and in what manner the
same is to be perforined, to be particularly described and ascertained in and by the
following statement :-
This process being based on new data it is necessary to make some preliminary
remarks in order to make clear the description that follows.
It has been proved that the amount of diastase which germinating grains contain
does not generally correspond in practice with the nominal aniount which should be
produced. theoretically a minimuin quantity of malt should by its yield of active
matters convert into saccharine a considerable quantity of amylaceous matter.
It is found on the contrary in practice that a relatively considerable quantity
of malt.must be used to arrive at even an imperfect degree of saccharification.
The cause of this phenomen is found to be in an impairing of the diastase through
the development of ferments which are harmful to it. Thus it is that malt worts
left, at the usual temperature for saccharification become gradually weaker, and
at the end of a longer or shorter, but always relatively short time, lose all their
activity.
The same phenomenon appears during the period of saccharification of amylaccous
matters by malt; the germs of the ferments, so abundant in germinating grains are
developed little by little in worts and gradually arrest the action of the diastase.
To remedy this difficulty it has been proposed to add to worts undergoing sacchari-
fication various acids, such as nitric, hydrochloric or sulphuric. These acids preserve
the worts more or less from alteration. Unfortunately the quantities of these acids
necessary to give this result weaken the diastase to a very considerable degree, and
the final result that nothing or very little, as regards saccharification, is gained by
their use.
The present modes of preserving the worts undergoing saccharification generally
consist of assisting them by means of the temperature and. by chemical agents not
favourable to the development of harmful feruients. But still the desired result has

page_text: not been attained, for on the one hand the worts are mixed with simple infusions of
malt. which. always contain ferments, and on the other hand the chemicals being
placed in a diluted material cannot act efficaciously and thus preserve the diastase
intact.
Taking these facts into consideration, it has been tried to purify malt by an
antiseptic which in weak doses should have no action on the diastase, while at the
same time it should destroy the gerins of other ferments.
In their researches my correspondents have discovered that hydrofluoric acid will
attain this result.
In fact by adding to a litre of infusion of malt, corresponding to about 200 to
300 grammes of malt, two or three drops of commercial hydrofluoric acid, it can be
preserved for 8 to 10 days without the liquid undergoing the least alteration or losing
any of its saccharifying principle.
My correspondents have besi les discovered that an infusion of malt acidulated by
hydrofluoric acid in the above named proportions has its maximum saccharifying
power at 25-30° C. and not at the temperature of 50-60° C. usually employed for
this purpose.
The preliminary purification of the malt by hydrofluoric acid allowed them to
obtain a very economical working, by which means they realised a very considerable
saccharification from a small quantity of malt.
Further, their first successes led them to apply the same principle to the fer-
mentation, and their experiments have shown them that hydrofluoric acid has a
very favourable action on the yeast, that it prevents the development of other ferments
and that its employment increases by this means very considerably the yield of
alcohol.
I. Preparation of infusion of malt and
extract.
diastase in the form of a concentrated
To crushed malt diluted with two or three times its volume of cold water is added
10 to 20 grammes of commercial hydrofluoric acid (containing about 20 per cent. of
pure hydrofluoric acid) for every hundred litres of the liquid, care must be taken
to keep the malt in suspension for some time.
This operation deprives the, malt of every germ of foreign ferments, and at the
same time produces a liquid quite suitable for employment as a liquefying, and
saccharifying agent. According to the amount of work which this liquor must
perform, the hydrofluoric acid is neutralised at the end of some hours, by means of
carbonate of lime or left as free acid, when the liquor must produce saccharification
in materials already containing lime salts.
Instead of employing as already shown the diastasic liquor, the dregs can also first
be separated so as only to preserve the amylin and the extract. This amylin and
extract can be used as they are, or they can be still further separated by filtration or
by decanting or by turbinage, and a clear or almost clear liquid is then obtained
which forms an unchangeable infusion. By evaporating this liquid in a vacuum at a
maximum temperature of 65-70° C. solid diastase is produced in the form of a
yellowish powder, an equal weight of which possesses a saccharifying action 25 to
30 times stronger than that of malt. The temperature of 65° C. must not be exceeded
when a product of a highly saccharifying power is to be obtained.
II. Manufacture of liquid syrups and of crystals.
As raw material, maize is employed by preference, although this mode of working
is adapted equally to starch and all other amylaceous materials. To maize steeped
or unsteeped, ground or unground, is added three or four times its volume of water
and it is then boiled under a pressure of three or four atmospheres for one or two
hours, by means of the usual apparatus. The boiling being finished the liquid is
cooled to 30 or 40° C. either by addition of cold water or by means of a refrigerator
at the surface or by any other mode. When brought to this temperature, the diluted
malt or the infusion with amylin or the clear extract of malt or even the solid diastase
prepared as detailed in the preceding paragraph 1 is added thereto.

page_text: The temperature of the liquid, after the addition thereto of the infusion, should
fall to 15 to 25° C., and it is then left for saccharification of which the duration may
vary from several hours to 48 hours according to the nature of the product it is
wished to obtain, and the quantity of dextrine it is wished to retain therein. If the
materials contain dregs in suspension as is the case with maize and cereals generally,
these dregs can, after two or more hours, be separated, either by means of a filter
press or by turbinage or by sifting, or by any other method generally employed.
The filtered liquor is then passed into the settling vats where the saccharification goes
on vigorously at a temperature of about 20° C.
According to whether it is wished to obtain a syrupy or solidified product, the
saccharification is arrested more or less quickly, the liquor is then boiled with a little
carbonate of lime. Afterwards the liquor is ovaporated at 38; to 42° Beaumé after
La preliminary filtration on any kind of filter.
II. Alcoholic fermentation. :
This system of making alcohol is based on the same method as that for the
manufacture of syrups as shown above.
Maize or other similar articles, with or without previous bruising, must be. thoroughly
crushed under pressure.:
:
:.
Diastase, with the addition of hydrofluoric acid as described above, is then added
in one of the forms and at the temperature named for the manufacture of syrups,
either in the form of concentrated. diastase or in the form of a clear infusion with
or without amylin, or finally in the form of ground malt.
As soon as the saccharification is thoroughly commenced, to the liquid, filtered or
not, yeast is added which has remained for several hours in contact with hydrofluoric
aci used at the rate of 15 to 20 gr: of acid of commerce (at about 20 per cent. of
pure acid) per hectolitre of liquid yeast.
The employment of a diastase agent and of a yeast very active and deprived of the
elements in them detrimental to alcoholic fermentation, allows of obtaining regularly
a return of 38 litres of alcohol, per 100 kilos of maize containing 63 per cent. of
amylin.
My correspondents have further. discovered in the .course. of their investigations
that commercial hydrofluoric acid in the proportion of 5 to 15 grammes per, hectolitre
of wort can be employed as a simple preservative and that without modifying in
the slightest any one of the ordinary processes: in use in manufactories. The addition
of hydrofluoric acid in the above named proportion can be, made before, during, or
after saccharification, before or after the addition, of the yeast and during the fer-
mentation and even before the boiling under pressure, in a given quantity which may
be even considerably increased if care be taken to correct the too great acidity after
boiling.
They have also found that the preservative action of hydrofluoric acid acts not only
on the diastase, but also on the yeast, preserving the latter, and that if care; bé taken,
during the saccharification of feculent and amylaceous substances, by acids, with the
view of obtaining alcoliol, to add to the worts, either before or after the saccharifica-
tion, before or after the addition of the yeast, or even during, the course of the
fermehtation, any quantity of hydrofluoric acid.up. to the point where fermentation is
possible, a much greater return than usual may be obtained.
On this subject it may be observed that, if, in the boiling of feculent and amylaceous
substances either with a view to the production of sugar starch or to alcoholic
fermentation; sulphuric, oxalic, hydrochloric. or other acids. generally used, be replaced
by commercial hydrofluoric acid, it suffices to employ 1 per cent. at most,. of this
latter to yield, at the end of one or two hours pressure of three atmospheres, wort
saccharified to at least. The point is very important as it means, the use of a
relatively very small quantity of acid and because the fluoride of calcium formed
during neutralization is much less soluble.than sulphate of lime and consequently is
éliminated more easily.
'
:
Especially in the case of the treatment of feculent and amylaceous substances with a

page_text: view to alcoholic fermentation, it. will be sufficient after boiling; to neutralize with
carbonate of lime up to a point. at: which it can be determined. by an experiment (test)
acidity. remrining is not in excess for the purpose of fermentation.
.
The same results are obtained ini the case of the fermentation of worts from beetroot
and molasses.. In the case. of molasses in. particular, my correspondents have
discovered that if instead of adding as usual about per centofi commercial hydrofluoric
acid per 100 kilos of molasses; a sufficient quantity of sulphuric acid be added to
render them slightly acid and that if care be taken besides; to add, any required
quantity of commercial hydrofluoric acid (and generally a quantity of 5 to 15 grammes
of commercial hydrofluoric acid per shectolitre of, wort: suffices) not only will a larger
yield of alcohol be obtained, but also.aumuch greater one of carbonate of potash than
is the case at present in the.production of alcohol by means of: sulphuric acid..
Finally they have found that in the treatment of any raw material for producing
alcoholic fermentation and yielding a residue utilisable in any manner, either for the
feeding of cattle or for any other purpose, if care. be taken either before, or after
distillation to add to the fermented worts or to the residue a quantity of about 5 to
15 grammes or more per hectolitresof: wort.or mash, the duration of their keeping is
greatly enhanced: this is of great importance for manufacturers of alcohol, especially
for those who have need to keep the residues for several days or for those who intend
to utilise them.
If.further care be taken, when the residue. is required for use, to add a small
quantity of lime, potash, soda, or even of any other alkalies or salts capable of
-neutralising the hydrofluoric acid, the article. is then rendered immediately available
without any change and similar to that produced only a few hours before.
i
By the addition of a stronger.dose of acid.it is possible to preserve the residue for
an almost indefinite time.
Having now particularly described and ascertained the nature of the said inven-
tion, and in what manner the same is to be performed, as communicated to me
by my foreign correspondents, I declare that what I claim is :-
1. The saccharification;tat:low temperature: (20-3° C.) of amylaceous sub-
stances: rendered industrially possible by the antiseptic action of hydrofluoric acid
-on: maltor, worts. in process of saccharification, this re-agent. being employed in the
proportions of 20 to 30 grammes.of. hydrofluoric acid to 100. litres of an infusion of
25 to 30 kilogrammes.of malt; this infusion being able to be rendered unchangeable
by the separation of the dregs- and the starch with the acid liquor and capable of
yielding solid diastase by the evaporation of the purified 'solution."
2. The application of the process set forth in claim 1 to the saccharification of any
amylaceous substance, the proportion of diastasic solution to be employed varying with
the nature of the substances to betsaccharified and the application of the same process
to alcoholic fermentation by the addition to the saccharifying matter of a suitable
quantity of yeast which has remained for. some hours mixed with hydrofluoric acid in
the proportions of 15 to 20 grammes:of acid per. hectolitre of yeast.
t
3. The use, in the process of fermentation of hydrofluoric acid in the quantity of
about 5 to 15 grammes of commercial acid per hectolitre of wort (and even in a larger
quantity for an acid fermentation) in the ordinary. mode of working in distilleries
where, feculent and amylaceous matters; as well as Jerusalem artichokes, are treated
either. by malt or by acids, and this at any period. of the manufacture either before
-the boiling, before. or after the saccharification. or even before, during or after the
addition of the yeast and at anyaphase of the fermentation whatever.
4. The use of hydrofluoric acid for the same object in the saccharification of grains
in the proportion of 1 per cent.sand more of commercial hydrofluoric acid per 100 kilos
of grains, neutralising afterwards this acid to the point required; for the fermentation.
5 The use of hydrofluoric acid in any given quantity either for acidulation.or
fermentation of substances like beetroot, cane molasses, or other s
sugar containing
**substances.
t.
1

page_text: 6. The use of hydrofluoric acid for the manufacture of starch sugar as described
above in paragraph 4, but neutralising it completely after saccharification.
7. The use of hydrofluoric acid in the quantity of 5 to 15 grammes and even more
of commercial hydrofluoric acid per hectolitre of wort and this before or after distil-
lation and with the object of making the residues less changeable or completely
unchangeable.
101 1
1000
WM. P. THOMPSON & Co.,
Agents for the Applicant.