IMPROVEMENTS IN THE TREATMENT OF HOPS FOR THE OBTAINMENT OF CERTAIN USEFUL PRODUCTS
Year: 1883

page_text: LETTERS PATENT to William Linden of Streatham Comnion in the County
of Surrey for an Invention of "IMPROVEMENTS IN THE TREATMENT OF HOPS
FOR THE OBTAINMENT OF CERTAIN USEFUL PRODUCTS
"
PROVISIONAL SPECIFICATION left by the said William Linden at the Office
of the Commissioners of Patents on the 13th August 1883.
WILLIAM LINDEN of Streatham Common in the County of Surrey,
"IMPROVE-
MENTS IN THE TREATMENT OF HOPS FOR THE OBTAINMENT OF CERTAIN USEFUL
PRODUCTS
">
This invention has for its object:
1) To prevent the unceasing deterioration of the hop flavour-essential oil—
in the hops in stock
•
2) To exhaust the hops of their valuable component parts for use in brewing
and other purposes.
3) To change the lupuline and resin which are insoluble in the wort into a
state soluble in the wort, water and alcohol.
4) To enable the brewer at all times to brew the finest flavoured kinds of beer
without the use of any kind of drugs, chemicals or finings, to flavour to bitter to
clarify, to preserve and to protect the same against acidity by means of the hop-
component parts alone viz: the essential oil, the lupuline, the hop-tannin and the
hop-resin.
By this invention I protect the brewer against tho great losses which he now
experiences through the unceasing oxidation of the flavor in the hops in stock and'
saves the amount of wort that now is retained in the hops after the hops are
boiled with it. The whole length of the wort can by my process be boiled with
the tannin and so perfectly clarify the same. A very good, paying bye product is
produced, viz: unbittered yeast which possesses on account of its great amount of
nitrogenous matter a greater feeding value than peas and beans.
For the purpose of soparating the essential oil of hops I subject (by preference
fresh green) picked hops to a process of distillation in a, preferably cylindrical,

page_text: steam jacket distilling apparatus the temperature of which should be from 125° C
to 175° C, until all essential oil is distilled over, steam being admitted to the inside
as well as to the jacket. The essential oil is now separated from the water and
put directly into bottles until quite full and with very accurately closing glass
stoppers. This constitutes the flavoring matter.
After this process of distillation the hops are brought into drying rooms and
exhausted of all humidity; the completely dried hops are now again put in the
before mentioned Steamjacket-distilling-apparatus and filled up with bisulphide
of carbon, so that the hops are perfectly covered with the bisulphide of carbon.
By admitting steam to the jacket the pan is warmed preferably to 40° C, that being
- below the boiling point of bisulphide of carbon, and when the bisulphide of carbou
is saturated, it is drawn off and this process of extraction is repeated as often as
required generally about 4 or 5 times, with fresh bisulphide of carbon until the
hops are perfectly exhausted of all their component parts which are soluble in
bisulphide of carbon. After the drawing off of the last extraction, the hops are
freed completely of the bisulphide of carbon by applying steam first to the jacket
only then to the inside of the apparatus also so as to drive over the last of the
vapour of bisulphide of carbon.
The whole of the extractions with bisulphide of carbon are now put in another
steamjacket distilling apparatus and the bisulphide of carbon completely distilled
off. The residuum after the distillation contains all the lupuline, the hop-myricine
_ and _hop resin Out of this mixture the lupuline and the hop resin are now
dissolved in alcohol, and by filtration the undissolved myricine is separated. The
alcohol is now separated by distillation from the dissolved lupuline and hop resin,
these are then treated with an aqueous solution of caustic potash or Soda until the
acid reaction is changed into a basic reaction. The quantity of caustic solution
I add is sufficient to convert the whole of the lupuline into lupulate but only a
portion of the resin into-resinate.
By these processes the bittering, the keeping, the preserving and the protecting
matters are obtained for the purpose of brewing.
For producing lupulate of potash or soda for medicinal purposes the hop resin
must be separated from the lupuline, therefore the before named mixture of lupulino
and hop-resin is dissolved in Ether and to the ether solution is added a saturated
aqueous solution of caustic potash or soda and this is to be repeatedly well shaken
until the caustic solution has a deep yellow colour. Then the lower aqueous layer
containing the resinate of potash or Soda must be separated and the other solution
must be repeatedly shaken with new portions of the caustic solution until the
yellow colour disappears.
The upper ether solution is after this to be shaken with distilled water to remove
tho Lupulate of Potash or Soda and this is repeated so long as the water has a 4
bitter taste.
The aqueous solutions are now concentrated or diluted according to the required
degree of strength to constitute the lupulato of potash or soda in solution for
medicinal purposes.
The residual hops after undergoing the processes before mentioned are now 4
with the addition of distilled water boiled out, generally 3 or 4 times, until the
hops are exhausted of their tannin. These boilings are carefully evaporated,
preferably in vacuo, to the state of a stiff extract which is the clarifying matter of
the hops, or hop-tannin,

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent filed by
the said William Linden in the Patent Office on the 13th February 1884.
WILLIAM LINDEN of Streatham Common in the County of Surrey "IMPROVE
MENTS IN THE TREATMENT OF HOPS FOR THE OBTAINMENT OF CERTAIN USEFUL
PRODUCTS
"
This invention has for its objects
1) To prevent the unceasing deterioration of the hop flavour-essential oil—in
the hops in stock.
2) To exhaust the hops of their valuable component parts for use in brewing
and other purposes.
3) To change the lupuline and resin which are insoluble in the wort into a state
soluble in the wort, water and alcohol.
:
4) To enable the brewer at all times to brew the finest flavoured kinds of beer
without the use of any kind of drugs, chemicals or finings, to flavour to bitter to
clarify, to preserve and to protect the same against acidity by means of the hop
component parts alone viz: the essential oil, the lupuline, the hop-tannin and tho
hop-resin
By this invention I protect the brewer against the great losses which he now
experiences through the unceasing oxidation of tho flavour in the hops in stock
and saves the amount of wort that now is retained in the hops after the hops are
boiled with it. The whole length of the wort can by my process be boiled with
the tannin and so perfectly clarify the same. A very good, paying bye product is
produced; viz unbittered yeast which possesses on account of its great amount
of nitrogenous matter a greater feeding value than peas and beans
For the purpose of separating the essential oil of hops I subject fresh green
picked hops to a process of distillation in a preferably cylindrical, steam jacket
distilling apparatus the temperature of which should be from 125° C to 175° C,
until all essential oil is distilled over, steam being admitted to the inside as well as
to the jacket.
The essential oil is now separated from the water and put directly into bottles
until quite full and with very accurately closing glass stoppers.. This constitutes
the flavouring matter.
For the said operation of distilling I prefer to employ a cylindrical still tho
height whereof is say 2, times the diameter, the centre of the bottom would be
somewhat depressed and fitted with a drawing-off cock. About 4 inches above
the bottom there is a false bottom which is perforated or constructed like a
strainer and in operation is covered by a straining cloth so that the hop seeds and
small particles may be retained when the liquid is run off from the still. As
mentioned the still is steam jacketted and steam can also be admitted into it. A
manhole is provided at a convenient height for the removal of the hops. The top
is closed hermetically by a lid from which a pipe leads to a cooling apparatus as
usual and there is in it an inlet closed when required by a cock and serving to
admit bisulphide of carbon as will horeinafter be described.
In the distilling operation steam is admitted both to the jacket and to the
interior of the apparatus.
After this process of distillation the hops are brought into drying rooms and
first exhausted of all humidity; the completely dried hops are now again put in
the beforementioned Steamjacket-distilling-apparatus and the latter filed up
with bisulphide of carbon, so that the hops are perfectly covored therewith. By

page_text: admitting steam to the jacket the pan is warmed preferably to 40° C; that being
below the boiling point of bisulphide of carbon, and when the bisulphide of carbon
is saturated with the substances soluble therein it is drawn off and this process of
extraction is repeated with fresh bisulphide as often as required generally about 4
or 5 times, until the hops are perfectly exhausted of all their component parts
which are soluble in bisulphide of carbon. After the drawing off of the last
extraction, the hops are freed completely of the bisulphide of carbon by applying
steam first to the jacket only then to the inside of the apparatus or pan also so as
to drive over the last of the vapour of bisulphide of carbon.
The whole of the extractions with bisulphide of carbon are now put in another
steam jacket distilling apparatus and the bisulphide of carbon completely distilled
off. The bisulphide still is similar in construction to that above described but its
height is equal to the diameter, it has no false bottom and only one steam pipe
communicating with its interior.
.
The residium after the distillation of the bisulphide contains all the lupuline, the
hop myricine and hop resin. Out of this mixture tho lupuline and the hop resin
are now dissolved in alcohol and by filtration the undissolved myricine is
separated. The alcohol is now separated by distillation from the dissolved lupuline
and hop resin, to these is added a saturated aqueous solution of caustic potash or
Soda and the mixture heated. This treatment is continued until the acid reaction
is changed into a basic reaction and the lupuline transformed into a lupulate of
alkali and some of the resin into resinato of alkali. The quantity of caustic solution
I add is sufficient to convert the whole of the lupulino into lupulate, but only a
portion of the resin into resinato.
By these processes the bittering, the keeping, the preserving and the protecting
matters are obtained for the purpose of brewing.
For producing lupulate of potash or soda for medicinal purposes the hop resin
must be separated from the lupuline, therefore the before named mixture of
lupuline and hop resin is dissolved in Ether and to the ether solution is added n
saturated aqueous solution of caustic potash or soda and this is to be repeatedly
well shaken until the caustic solution has a deep yellow colour. Then the lower
aqueous layer containing the resinate of potash or Soda must be separated and the
ether solution must be repeatedly shaken with new quantities of caustic solution
until the yellow colour disappears viz: as long as the caustic solution can take up
any resin
The upper ether solution is after this to be shaken with distilled water to
remove the lupulate of potash or soda and this is repeated so long as the water
take a bitter taste.
The aqueous solutions are now concentrated or diluted according to the required
degree of strength to constitute the lupulato of potash or soda in solution for
medicinal purposes.
The residual hops after undergoing the process before mentioned aro now with
the addition of distilled water boiled out generally 3 or 4 times, until the hops are
exhausted of their tannin. These boilings are carefully evaporated, preferably in
vacuo, to the state of a stiff extract which is the clarifying matter of the hops, or
hop-tannin.
By my invention I obtain not only the advantages herein above referred to but
the bop-constituents will also be readily stored and transported; the solubility of
these materials allows any desired taste and flavour of the beer to be obtained
irrespective of the amount of alcohol contained therein; the resinate of alkali
moreover counteracts souring of the beer as when the free resin is all oxidised and
acidity begins to be produced it will in its nascent state attack the resinate and
combine with the alkali this being specially important with light beer and in
warm seasons, The yeast obtained from brewing when my invention is used
being very rich in nitrogenous matters will with suitable additions form a valuable
food readily taken by cattle and fowls

page_text: Moreover the Myricine being insoluble in alcohol it is an advantageous feature
of my invention that this matter is eliminated.
Having now described the nature of the said invention I wish it to be understood
that I am aware that the employment of some parts of the process above set forth
have ere this been proposed and to such parts I lay no claim but what I claim is:
First The complete process substantially as described for extracting and
preserving the constituents of hops for the purpose of rendering the same
soluble, permanent and lastingly useful.
Second. The preparation for brewery purposes of a material consisting of
lupuline resin and an alkali and soluble in wort, water and alcohol substantially
as described.
Third The preparation of lupulate of alkali or of solutions thereof for medicinal
purposes, substantially as set forth.
In witness whereof I the said William Linden have hereunto set my hand and
seal this thirteenth day of February in the year of Our Lord one thousand eight
hundred and eighty four.