IMPROVEMENTS IN TREATING JAPAN AND OTHER VEGETABLE WAX
Year: 1859

page_text: LETTERS PATENT to Warren De la Rue, Manufacturer, and Dr. Hugo
Müller, both of No. 110, Bunhill Row, in the County of Middlesex,
for the Invention of "IMPROVEMENTS IN TREATING JAPAN AND OTHER
VEGETABLE WAX."
Sealed the 27th October 1859, and dated the 11th August 1859.
PROVISIONAL SPECIFICATION left by the said Warren De la Rue and
Dr. Hugo Müller at the Office of the Commissioners of Patents, with
their Petition, on the 11th August 1859.
We, WARREN DE LA RUE, Manufacturer, and Dr. Hugo MÜLLER, both of
110, Bunhill Row, in the County of Middlesex, do hereby declare the nature
of the Invention for "IMPROVEMENTS IN TREATING JAPAN AND OTHER VEGETABLE
WAX," to be as follows:-
This Invention has for its object improvements in treating japan and other
vegetable wax. For these purposes the japan or other vegetable wax is
dissolved by a suitable solvent, and then separated into different products.
The solvents employed are hydrocarbons and alcohal, or wood spirit is used to
precipitate or separate different products. The solvents employed may be re-
obtained, and again and again used.

page_text: SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said Warren De la Rue and Dr. Hugo Müller in the Great Seal
Patent Office on the 11th February 1860.
TO ALL TO WHOM THESE PRESENTS SHALL COME, we, WARREN
DE LA RUE, Manufacturer, and Dr. HUGO MÜLLER, both of No. 110, Bunhill
Row, in the County of Middlesex, send greeting.
WHEREAS Her most. Excellent Majesty Queen Victoria, by Her Letters
Patent, bearing date the Eleventh day of August, in the year of our Lord
One thousand eight hundred and fifty-nine, in the twenty-third year of Her
reign, did, for Herself, Her heirs and successors, give and grant unto us, the
said Warren De la Rue and Hugo Müller, Her special licence that we,
the said Warren De la Rue and Hugo Müller, our executors, adminis-
trators, and assigns, or such others as we, the said Warren De la Rue
and Hugo Müller, 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. "IMPROVEMENTS IN
TREATING JAPAN AND OTHER VEGETABLE WAX," upon the condition (amongst
others) that we, the said Warren De la Rue and Hugo Müller, our executors
or administrators, by an instrument in writing under our or their hands
and seals, or under the hand and seal of one of us or them, 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 imme-
diately after the date of the said Letters.Patent.
NOW KNOW YE, that we, the said Warren De la Rue and Hugo
Müller, do hereby declare the nature of the said Invention, and in what
manner the same is to be performed, to be particularly described and ascer-
tained in and by the following statement thereof, that is to say:-
This Invention has for its object improvements in treating japan and other
vegetable wax. For these purposes the japan or other vegetable wax is
dissolved by a suitable solvent, and then separated into different products.
The solvents employed are hydrocarbons and alcohol, or wood spirit is used to
precipitate or separate different products. The solvents employed may be re-
obtained, and again and again used.
Having thus stated the nature of our Invention, we will proceed more fully
to described the manner of performing the same.

page_text: In order that the process may be more readily understood, we here state.
that, the so-called Japanese wax, and other similar substances, consist of
several components, which, from their different degrees of solubility in certain
menstrua, admit of being separated the one from the other without its being
necessary to effect their partial decomposition by saponification, distillation, or
other means usually practised to render such waxy or fatty bodies more.
applicable to the manufacture of candles and lubricants.
Japanese wax as imported into this country is generally in the form of cakes
of various sizes, it is of a yellowish white color, and resembles bleached bees'--
wax, but is more brittle than bees'-wax at ordinary temperatures, yet becomes
softer and more sticky when kneaded between the fingers.
Japanese wax consists of a solid, hard, and colourless fatty substance, a soft
semi-fluid fatty substance, and a small proportion of a resinous body; under
no conditions of temperature can these constituents be separated by mechanical
pressure. The object of our Invention is to effect their separation by means
of solvents, either capable of dissolving the whole fat at a certain temperature,
and of yielding up one constituent after the other as the temperature falls, or.
of solvents capable of removing one constituent to the exclusion of the
others.
The solvents we employ are the following:-1st, the hydrocarbons boiling
between 176° Fahrenheit and 392° Fahrenheit, obtained in distilling Burmese
naphtha and petroleums generally; 2nd,.the.hydrocarbons obtained in distilling
coal, bog-head coal, bituminous shale, lignite (wood coal), or peat, using, by
preference, such as boil below 212° Fahrenheit up to 392° Fahrenheit;.
3rd, alcohol which may now be obtained as methylated spirit, at a sufficiently
low price to admit of its application very generally in the arts; or wood spirit
(naphtha).
As the solvent powers of the above fluids differ considerably, the process for
treating Japanese and other similar substances must be varied according to
the nature of the solvent. We may at once state that those hydrocarbons
which are derived from coal tar and boghead coal, bituminous shale, wood
coal, or lignites, or peat consist, in a great measure, of those hydrocarbons
known to chemists as members of the benzole series, and we find that they are
the most powerful solvents for Japanese wax and similar bodies. The hydro-
carbons extracted from Burmese naphtha (and similar petroleums) consist
principally of another series of hydrocarbons, distinguished by chemists as the
hydrurets of the organic radicals of the methyl series; these hydrocarbons we.
find are much less powerful solvents. Lastly, alcohol, methylated alcohol, or
metbylic spirit (wood spirit or naphtha) we find dissolve scarcely any of the

page_text: solid fat at ordinary temperatures, but on the other hand, freely dissolve the
semi-fluid fat and the resinous body.
We will commence by describing the employment of alcohol for the
separation of the different constituents of Japanese wax or other similar
bodies. In order to do this we avail ourselves of the solvent power of alcohol,
methylated spirit or wood [spirit, or naphtha, and we take such spirit as
contains as little water as possible, but it is not essential that alcohol absolutely
free from water should be used, and it would not be economical to do so.
We take three to four parts by weight of the solvent, and having placed this
in a digesting vessel, we add thereto one part by weight of the wax and raise
the temperature until the liquid rapidly boils, so as to produce agitation during
the operation, and we continue the rapid boiling for about an hour, the
digester being connected with a condenser, which condenses the alcoholic or
other vapours, and returns the condensed alcohol, &c. We draw off the liquor
from the digester, and allow it to cool, when a small portion of solid fat
deposits, which is added to the undissolved fatty mass. This undissolved fatty
mass is nearly free from the semi-fluid fat and the resinous body, which
remain dissolved in the alcohol even when cold. The solid fat is sufficiently
pure for use, but may be further purified, if desired, by a second digestion with
boiling alcohol or wood spirit, or naptha. The semi-fluid fat, together with
the resinous body, is obtained on distilling off the greater part of the alcohol
or wood spirit, or naptha, and finally removing the last traces of solvent by
blowing steam through it; it is valuable as a lubricant, or may be used for the
production of soaps.
The petroleuum oils we employ in two different ways; the first is similar to
that of the alcohols, and consists in the removal of the semi-fluid fat and resin
from the solid fat; the second consists in a method of separating the solid fat
by a process of crystallization from a solution of the entire Japanese or other
similar wax.
Firstly, we break in small pieces or plane into thin shavings the Japanese
wax, and having placed it in a closed funnel-shaped vessel, with a draw-off
cock in the bottom; we saturate the powdered wax with Burmese or other
petroleuum hydrocarbon, and having allowed it to remain in contact with the
wax for some hours, we run carefully a layer of fresh hydrocarbon on the
surface, and then open the tap at the bottom of the funnel, and allow the
saturated bydrocarbon to run off; this contains principally the semi-fluid fat.
The fresh hydrocarbon, by displacement, comes in contact with the wax, and
after some hours dissolves a further quantity of semi-fluid fat, and also a
portion of the solid fat; in its turn it is drawn off, and the residual solid fat is

page_text: washed with a further portion of the hydrocarbon, and after being melted and
subjected to a stream of steam to volatilize any residual hydrocarbon is fit for
use. A further quantity of solid fat requiring to be afterwards purified, may
be obtained from the oily solution on distilling off a part of the petroleuum oil,
and cooling. The semi-fluid fat is obtained on completely distilling off the
petroleuum oil in a stream of steam.
Secondly, we add to the unbroken Japanese wax or other similar body
twice its weight of Burmese or other petroleuum hydrocarbon, and heat it to a
temperature of about 155° Fahrenheit; the wax first melts, and then com-
pletely dissolves, leaving a slight residue of foreign matter, which is allowed to
deposit.
..
The clear solution is allowed to cool gradually, and when about one-third of
the wax employed has crystallized out, the mother liquor is drawn off, and is
allowed to cool still further, when a second deposit forms in all respects similar
to the first, and when no further crystallization takes place the mother liquor
is again drawn off. The two lots of crystals are now placed in a draining.
vessel and washed with a saturated petroleum oil solution of the solid fat,
purified by a previous operation, in order to completely remove all traces of
the semifluid fat. The so washed solid fat is now subjected to the action of a
current of steam, to remove all traces of hydrocarbon, and on cooling it
solidifies, and is fit for use. The semi-fluid fat is obtained on distilling off the
solvent, and a small further portion of the solid fat is obtained by conducting
the distillation by a series of steps, and allowing the fatty solution to cool
between each step.
When benzole hydrocarbons (coal naphthas, shale naphthas, &c.) are
employed we have found it expedient to employ these vehicles in connection
with alcohol or wood spirit, the alcohol or wood spirit being employed to aid
in precipitating or separating the different products, which is the second
use of alcohol or wood spirit alluded to in our Provisional Specification.
We take two parts by weight of the benzole hydrocarbon to one part by
weight of Japanese wax or other similar substance, and dissolve the wax by
the aid of a gentle heat (110° Fahrenheit); we then add to the solution one-
fifth of its volume of strong alcohol or wood spirit. The solution is allowed to
acquire the temperature of the air, when the greater part of the solid fat
deposits, the mother liquor is drawn off and again heated to about 100°
Fahrenheit, and a fresh and similar quantity of alcohol or wood spirit is added.
On cooling the liquor deposits a fresh quantity of the solid fat; these two portions
of solid fat are treated in the same way as has been described when Burmese
or other petroleum naphtha was employed. The mother liquid still contains

page_text: some solid fat, which is at once precipitated on the addition of a further
quantity of alcohol, &c. to the cold solution, but not being so pure as the first.
deposits, it is added to the original wax in future operations. The semi-fluid
fat is obtained together with the resinous substance from the mother liquor in
the following manner :-Water is added to the alcohol hydrocarbon solution,:
which removes the alcohol, the supernatant hydrocarbon retaining in solution
all the fatty body, the dilute alcohol being drawn off the hydrocarbon solution
of the fat is subjected to the action of a current of steam, by which means the
hydrocarbon is distilled off, the semi-fluid wax remaining in the still.
The solid fat is applicable to the manufacture of candles; by itself it gives
a comparatively weak flame, and is particularly valuable for admixture with,
paraffin or other light-producing substances, which have a tendency to give a
smoky flame, as it remedies. this defect without lessening the hardness of the
candle.
What we claim is, the employment of hydrocarbons and alcohol, &c., as
enumerated for treating Japan or other vegetable wax in the manner described;
we do not, however, confine ourselves to the precise proportions given, as they-
admit of being varied, as does also the temperature at which the operations are.
conducted.
In witness whereof, we, the said Warren De la Rue and Hugo Müller,
have hereunto set our hands and seals, this Eleventh day of February,
in the year of our Lord One thousand eight hundred and sixty.
WARREN DE LA RUE
WARREN DE LA RUE. (16)
HUGO MÜLLER.
(L.B.)