Improvements relating to the Manufacture of Spirit from Grain and Cereals and to the Treatment of the Bye-products derived there- from for the Production of Cattle Food, Charcoal, and Manure.
Year: 1889

page_text: Date of Application, 15th Sept., 1889
Complete Specification Left, 12th June, 1890-Accepted, 12th July, 1890
PROVISIONAL SPECIFICATION.
Improvements relating to the Manufacture of Spirit from Grain and
Cereals and to the Treatment of the Bye-products derived there-
from for the Production of Cattle Food, Charcoal, and Manure.
I ALEXANDRE MANBRÉ Senior of 13 Osborne Terrace, Clapham Road in the
County of Surrey Brewer and Sugar Manufacturer do hereby declare the nature of
this invention to be as follows:-
My invention relates to an improved process of producing or manufacturing spirit
from grain and cereals in which process the materials are treated in a manner that
produces much better results than live hitherto been obtained from their use, and
the distilled spirit and bye-products obtained are of much superior character as
compared with those hitherto produced.
By the present process of producing or manufacturing spirit known in the trade as
grain or neutral spirit the chief materials used are maize, barley, oats, rice and malt,
the malt acting as a saccharifying agent. These materials are at first subjected to .
process of crushing or grinding to be reduced into meal. This meal, which is a
mixture of starch, husk, bran, cellulose, nitrogenous matters and other constituents
mingled together, is then subjected to a mashing process & through the agency of
malt, water and heat (the temperature usually used varying from 140° to 180°
Fahrenheit) is converted into a saccharine extract called wort which wort in its crude.
and impure condition is then cooled down to a suitable temperature and subjected to
fermentation, and the resulting spirit is then distilled off leaving bye-products known
as grains, dregs and wash.
The spirit thus produced is more.or less contaminated with an acrid empyreumatic
flavour known as fusil oil which considerably lessens the quality and value of the
spirit. This defective result is chiefly due to the deficiency of the heat or tempora-
ture used in the process of saccharification which temperature although of sufficient
power to convert the matured starch into suitable alcoholizable saccharine is on the
contrary insufficient to effect the like result from the unmatured starch which
amounts to from 5 to 20 per cent., this unmatured starch being metely converted
partly into amids the nutriont of germs of disease and partly into a liquid acrid
extract which by reacting on the amids, fatty and other deleterious matters, generates
the empyreumatic flavour imparted to the spirit; and the bye-products which are also
contaminated and impregnated with the said amids, ferments of disease and acrid
flavour are likewise deficient in quality and properties as a nutrient for cattle food
and owing to their being impregnated with a large proportion of acrid moisture
unless they are consumed within a few days of their production they undergo rapid
decomposition and as a consequence are then unfit for food.
Another process is also in use for the purpose of obtaining an increased yield of
spirit and the neutralization of the acrid and empyreumatic flavours, the saccharifica-
tion of grain and cereals being effected by means of sulphuric acid, but owing to
carbonate and quick lime being used to neutralize the said acid, sulphate of lime is
formed, but as sulphate of lime also possesses an acrid and bitter flavour, this acrid.
and bitter flavour is imparted to the spirit which greatly lessens its quality and
value and the bye-products obtained, being also impregnated and saturated with the
bitterness and acridity of the sulphate of lime with which they are inixed and
incorporated, are likewise of little value as cattle food.
An attempt has also been made to use a compound of phospho-sulphate of line
as a substitute for sulphuric acid in the process of saccharification, but as the tem-
perature used in the process amounts to from 250 Fahrenheit to 300 Fahrenheit and
that by experience it has been found that phosphoric acid evaporates at 212 Fahrenheit

page_text: the resultant is that 'the said phosphoric acid being thus liberated or otherwise
separated from the said compound, sulphate of lime only remains as a reacting agent
the power of which is not sufficient to attain the object aimed at.
Now I have found that by employing my improved process of treating the materials
used and selecting the proper agents & heat in the manner hereinafter described I am
enabled to produce spirit of the greatest purity free from empyreumatic flavour and
I am also enabled to produce from the bye-products a most valuable and nutritious
food of great stability specially suitable for horses, cattle, cows, calves, lambs, sheep,
poultry, pigs &c. This food being particularly valuable for its fat and muscle
forming properties owing to the large proportion of phosphates and other nutritious
constituents it contains and as it is specially prepared and made into a cake com-
pressed by special powerful hydraulic engines and rendered almost free from
moisture it can be kept in stock any length of time without deteriorating or losing
any of its nourishing properties. It is therefore most suitable for transport and for
exportation; and lastly, I also produce charcoal and manure of superior quality.
In carrying out my new improved process I proceed as follows:-
I use, as converting agents, malt and sulphuric acid in a manner that has not
hitherto been put in practice, the malt being merely employed to act as a preparatory
converting agent for modifying the starch towards solubility and to start its conversion
into amids and dextring, the sulphuric acid being employed to completed the conver-
sion of the amids and dextrine into alcoholizable saccharine.
I then proceed in the following manner:
I grind the grain, cereals and malt selected to be used into a fine meal and remove
the nusk or bran therefrom which husk or bran is kept aside or in reserve to be
hereafter mixed with the other bye-products. I then dilute the meal (using only
2 to five pounds weight of malt meal for every hundred pounds weight of the grain
meal) into about two thirds of the quantity of water it is intended to use and I heat
the mixture of meal and water until it reaches 180 Fahrenheit at which temperature
the starch from the meal is thoroughly dissolved and partly converted into aids and
partly into dextrine. I then introduce the said partly converted meal mixture into a
closed vessel (by preference made of copper or gun metal and capable of resisting an
internal pressure of from 90 to 100 pounds to the square inch) in which vessel the
remaining third portion of the water intended to be used (mixed together with from
2 to 3 pounds weight of sulphuric acid for every hundred pounds weight of meal
used) bas also been heated to 180 Fahrenheit and when the two said mixtures are
thus collected together into the said closed vessel the temperature is raised to from 300
to 320 Fahrenheit at which temperature it will be found that the conversion of the
starch into alcoholizable saccharine is fully completed. I then neutralize the
sulphuric acid by phosphate of lime thus forming a compound of sulpho bi-phosphate
of lime which compound in combination with other albuminous and nitrogenous
matters acts most effectually in obtaining by fermentation the full conversion of the
saccharine into a full flavoured spirit of the greatest purity free from empyreumatic
flavour and in its character of a co-bye-product, this compound being one of the
chief constituents of a nutrient for cattle will in combination with the other bye-
products considerably increase the nutritious properties of the food.
The neutralized saccharine solution is then drawn off into a draining vessel,
allowed to drain off, cooled down & subjected to alcoholic fermentation as usual.
The bye-products left in the draining vessel are then treated in the following
manner for producing cattle food, the husk or bran kept in reserve is added to the
bye-products & well mixed together with a suitable proportion of any one or more of
the following articles of food namely:-Oat meal, barley meal, rye meal, maize
meal, wheat bran, linseed oil cake &c. as may be found most suitable to the peculiar
wants of horses, cattle, cows, calves, lambs, sheep, poultry, pigs &c. which mixture is
then subjected by preference to powerful hydraulic pressure to eliminate the moisture
it contains the final result being a compressed.cake.ready for use.
The bye products derived from the fermentation of the saccharine into alcohol are
treated in the same manner.

page_text: For the production of charcoal, I subject the compressed bye-products (but without
the addition of the articles of food hereinbefore enumerated) to the process of
calcination resulting in the production of charcoal of superior quality most suitable
for the trade whether mixed or not with other charcoal.
And for the production of manure I grind the compressed bye-products into meal
which then mix in a suitable proportion with any other manure products such as
nitrates phosphates and ammoniacal preparations.
Dated this 18th day of September 1889.
COMPLETE SPECIFICATION.
Improvements relating to the Manufacture of Spirit from Grain and
Cereals and to the Treatment of the Bye-products derived there-
from for the Production of Cattle Food, Charcoal, and Manure.
I ALEXANDRE MANBRÉ Senior of 19 Warwick Terrace, Vicarage Lane, West Ham
in the County of Essex formerly of 13 Osborne Terrace, Clapham Road in the County
of Surrey, Brewer and Sugar Manufacturer 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 :-
My invention relates to an improved process of producing or manufacturing spirit
from grain and cereals in which process the materials are treated in a manner that
produces much better results than have hitherto been obtained from their use and
the distilled spirit and bye-products obtained are of much superior character as
compared with those hitherto obtained.
By the present process of producing or manufacturing spirit known in the trade
as grain or neutral spirit the chief materials used are maize, barley, oats, rice, and
malt, the malt being specially used as a saccharifying agent. These materials are at
first subjected to a process of crushing or grinding to be reduced into meal. This
meal, which is a mixture of starcb, husk, bran, cellulose, nitrogenous and albuminous
matters and other constituents mingled together is then subjected to a mashing
process and through the agency of malt water and heat (the temperature usually used
varying from 140° to 180° Fahrenheit) is converted into a saccharine extract called
wort which wort in its crude and impure condition is then cooled down to a suitable
temperature and subjected to fermentation and the resulting spirit is then distilled
off leaving bye products known as grains dregs and wash, the spirit thus produced is
more or less contaminated with an acrid empyreumatic flavour known as fusel oil
which considerably lessens the quality and value of the spirit. This defective result
is chiefly due to the deficiency of heat used in the process of saccharification, the
temperature although of sufficient power to convert the matured starch into suitable
alcoholizable saccharine being insufficient to effect the like result from the unmatured
starch which amounts to from 5 to 20 per cent. of the whole according to the degree of
maturity of the grain and cereal used. This unmatured starch is converted partly into
amids the nutrient of germs of disease and partly into a soluble acrid extract which by
reacting on the amids and fatty and other deleterious matters generates the
empyreumatic flavour (fusel oil) in the spirit. The bye-products which are also
contaminated and impregnated with the said amids, ferments of disease and acrid
flavour are deficient in quality and properties as a nutrient for cattle food and
owing to their being impregnated with a large proportion of acrid moisture they
undergo rapid decomposition unless they are consumed within a few days of
their production and as a consequence become unfit for cattle food.
In another process used for the purpose of obtaining an increased yield of spirit
and the neutralization of the acrid and empyreumatic flavours the saccharification of
grain and cereals is effected by means of sulphuric acid, but owing to carbonate of
lime and quick lime being used to neutralise the said acid sulphate of lime is formed
and this also possesses an acrid and bitter flavour, which is imparted to the spirit and
greatly lessens its quality and value: The bye-products obtained by this process are

page_text: also impregnated with the bitterness and acridity of the sulphate of lime with which
they are mixed and are likewise of little value as cattle food.
Attempts have been made to use a compound of phospho-sulphate of lime as a
substitute for sulphuric acid in the process of saccharification; but as the
temperature used in the process is from 250° to 300° Fahrenheit and as phosphoric
acid. evaporates at 212° Fahrenheit the result is that the phosphoric acid, being
thus liberated or otherwise separated from the compound phospho-sulphate of lime,
only remains as a re-acting agent, the power of which is not sufficient to attain
the object aimed at.
Now by my improved process of manufacturing spirit from grain and cereals and
trenting the bye-products derived therefrom for the production of cattle food
charcoal and manure I have found that by treating the materials used and select-
ing the proper agents and heat in the manner hereinafter described I am enabled
to produce spirit of the greatest purity free from empyreumatic flavour (fusel oil)
and I am also enabled to produce from the bye-products a most valuable and
nutritious cattle food of great stability in composition suitable for horses, cattle,
cows, calves, lambs, sheep, poultry, pigs &c. This cattle food is particularly
valuable for its fat and muscle forming properties owing to the large proportion
of phosphates and other nutritious constituents which it contains. It can be made
into a cake compressed by hydraulic or other machinery and rendered almost free
from moisture and thus it can be kept in stock for any length of time without
deteriorating or undergoing decomposition or losing any of its nourishing properties.
It is therefore most suitable for transport and for exportation. By my new process
I also produce charcoal and manure of superior quality.
In carrying out my new improved process I proceed as follows:-
1 use as converting agents germinated barley known as malt and sulphuric acid
in a manner that has not hitherto been put in practice. The barley malt is
employed in the manner hereinafter described merely as a preparatory converting
agent for rendering more soluble the starch contained in the grain and cereals and
to start its conversion into amids and dextrine. The sulphuric acid is employed to
complete the conversion of the amids and dextrine into alcoholizable saccharine and
to vaporize the fusel oil contained in the grain cereals, and malt. I proceed in the
following manner :-
I grind separately the grain cereals and malt selected to be used into a fine meal
flour and remove the husk bran and cellulose therefrom which husk bran and
cellulose are kept aside or in reserve to be used as hereinafter described, I then dilute
the selected proportions of grain cereals and meal flour intended to be used with
about two thirds of the quantity of water which it is intended to use, adding to the
mixture from two to five pounds of malt meal flour for every hundred pounds weight
of grain cereals and meal flour used. I then heat the said mixture of meal flour and
water (which must be stirred all the time) until it reaches 180° Fahrenheit, at which
temperature the starch is thoroughly dissolved and converted partly into amids partly
into dextrine and partly into maltose. I then introduce this partly converted meal
mixture into a closed vessel (made by preference of copper or gun metal and capable
of resisting an internal pressure of from 90 to 100 lbs. to the square inch) in which
yessel the remaining third portion of the water intended to be used (mixed together
with from 2 to 3 pounds weight of sulphuric acid for every 100 lbs, weight of grain.
and cereal meal flour used) has been heated to 180 degrees Fahrenheit. The vessel
is then closed and the temperature is raised to from 300° to 320 degrees Fahrenheit
at which temperature it will be found that the conversion of the starch into alcoholiz-
able saccharine is fully completed. I then neutralize the sulphuric acid by phosphate
of lime thus forming a compound of sulpho-phosphate of lime, which compound in
combination with the albuminous and nitrogenous matters acts most effectually in
obtaining by fermentation the full conversion of the saccharine into a full flavoured
spirit of the greatest purity free from empyreumatic flavour. This compound, being
one of the chief constituents of a nutrient for cattle, considerably increases the
nutritious properties of the bye products as a food.

page_text: The neutralized saccharine solution is then subjected to a process of filtration and
when separated from the residuum is then cooled down and subjected to alcoholic
fermentation as usual and the spirit produced is then distilled off.
As regards the treatment of the bye-products for the production of cattle food
charcoal and manure the foregoing shews that three kinds of bye-products are
obtained which number 1, 2 and 3. No. 1 being the husk bran and cellulose
derived from the grinding of the grain cereals and malt No. 2 being the residuum
derived from the filtration of the neutralized saccharine solution and No. 3 being
the residuum derived from the alcoholic fermentation of the saccharine solution and
distillation of the spirit produced.
For the production of cattle food I proceed as follows:-I treat the three bye-
products by mixing them either separately or together as may be found most suitable,
with a suitable proportion of any one or more of the following food materials namely:
oat meal, barley meal, rye meal, maize meal, wheat bran, linseed oil cake &c. as
may be found most suitable to the peculiar wants of horses, cattle, cows, calves,
lambs, sheep, poultry, pigs &c. which mixture is then subjected to powerful pressure
(by preference hydraulic) of from 200 to 300 tons to eliminate the moisture it
contains, the final result being a compressed cake ready for use.
For the production of charcoal I subject the said bye products either separately
or together to a like process of compression but without the addition of the food
materials above mentioned. The compressed bye-products thus obtained are then
ground into a fine meal and subjected to the process of calcination in the usual way
the result being the production of a charcoal of a superior quality.
For the production of manure I subject the bye products either separately or
together to a like process of compression. The compressed bye-products are then
ground into a fine meal which I mix in any suitable proportions with any other
manure products such as phosphates, nitrates, ammoniacal preparations and cattle
manure according to requirements.
I may remark that the aforesaid No. 1 bye product when mixed with a suitable
proportion of oat meal is specially suitable and most valuable for horses food No. 1
and No. 2 when mixed with suitable proportions of any one or more of the food
materials hereinbefore mentioned are specially suitable and most valuable for all
classes of cattle and poultry food and No. 3 whether mixed with other food materials
or not is specially suitable and most valuable for pigs food.
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
First. In the manufacture of spirit from grain and cereals the improved process
of effecting the complete saccharification of the starchy matters contained in the
grain and cereals by first subjecting the said starchy matters to a preparatory
conversion, through the action of malt and secondly through the action of sulphuric
acid and high heat in a closed vessel substantially as herein described.
Second. Neutral spirit produced from grain and cereals by the process hereinbefore
described and claimed.
Third. Cattle food charcoal and manure manufactured from the bye products
produced in the manufacture of spirit by the process herein before described and
claimed.
Dated this Twelfth day of June 189n
ALEXANDRE MANBRÉ, SENIOR.