Improvements in the Manufacture of Sugar and in the Apparatus Employed therein.
Year: 1893

page_text: Date of Application, 20th July, 1893
Complete Specification Left, 21st May, 1894-Accepted, 15th Sept.,
1894
PROVISIONAL SPECIFICATION.
Improvements in the Manufacture of Sugar and in the Apparatus
Employed therein.
I, JAMES YATE JOHNSON of 47 Lincoln's Inn Fields, in the County of
Middlesex, Gentleman, do hereby declare the nature of this invention (which
has been communicated to me from abroad by Jean Ercole Pellegrini of Calle
Cazanova 75 and 77 Barcelona in the Kingdom of Spain, Chemist) to be as
follows
This invention relates to the manufacture of sugar and enables a crystallisable
sugar to be produced by the synthesis of carbonic acid ethylene or other hydro-
carbon and water as hereinafter explained the said synthesis being preferably
performed by the action of endosmose for which purpose I prefer to employ a
specially constructed apparatus provided with diaphragms or partitions composed
of pumice stone prepared and arranged as hereinafter more fully set forth.
The process for the manufacture of crystallizable sugar by synthesis according
to this invention is based upon the combination of carbonic acid ethylene or other
hydrocarbon and water brought together under special conditions and in the
proportions indicated by the formula 4 CO', 4 C'H', 3 H2O) representing the
composition of crystallizable sugar.
Endosmose constitutes an example of the means which may be employed in
practice for effecting the synthesis of these three constituents of crystallizable sugar
and is employed by preference in carrying out this invention with the aid of a
specially constructed apparatus.
This apparatus is provided with a block of porous material preferably in the
form of a cube composed of pumice stone which is a highly porous material and
very readily permeated by gases. In this cube are formed numerous deep holes
or passages which do not pass completely through the block but extend from
each side to within say about 8 inches from the opposite side. These passages
are about one eighth of an inch in diameter and are parallel with one another.
This cube is carefully washed firstly with water acidulated with sulphuric acid
and afterwards with water alone until all traces of acid have disappeared. After
drying it carefully in a stove it is boiled for about one hour in a solution of
bi-chloride of platinum which has the effect of increasing the porosity of the
pumice stone; the cube is afterwards calcined in a muffle furnace heated to
redness.
When the cube has cooled it is placed in a box or case of cast iron or other
suitable material of an internal length three times greater than the side of the
cube but the width and height of which are exactly equal to the said side. The
cube or stone is placed in the middle of this box with the parallel passages in a
horizontal position and extending in the direction of the length of the said box. The
cube is retained in position between two steel plates perforated with holes registering
exactly with the holes in the stone so that the gases which as hereinafter explained
are supplied to two chambers on each side of the block enter the passages formed in
the said block.
The interior of the case or box is preferably nickel plated and planed and is
hermetically closed so as to prevent any leakage of gas. At the two ends the
case communicates with tubes supplying carbonic acid and a hydrocarbon such
as ethylene respectively. Each tube is provided with means for regulating the
proportions of the gases and consisting of a meter for measuring the volume, a
gauge indicating the pressure and a regulating valve. A pipe provided at the

page_text: upper part of the apparatus supplies steam through two branches communicating
with the upper part of the chambers on each side of the pumice stone.
This pipe is provided with a valve for regulating the quantity of steam supplied
to the apparatus. The underside of the box or case likewise communicates with two
branch pipes enabling the said chambers to be emptied through a passage provided
with a discharge valve.
In working this apparatus these valves are closed and the regulating valves are
opened.
The hydrocarbon is then forced under pressure into one of the compartments
and carbonic acid is similarly supplied to the other compartment. By means
of the regulating devices herein before referred to the supply of the two gases
is regulated in such a manner that they are forced into the apparatus in equal
volumes.
After a few moments the steam supply valve is opened and steam under a
pressure equal to that of the hydrocarbon and carbonic acid is introduced into
the chambers or compartments on each side of the perforated block or pumice
stone.
The apparatus becomes rapidly heated and is supplied with the gases during
about half an hour. The gases mix by endosmose through the substance of the
pumice stone and on the expiration of this time there is extracted through the
discharge valve a syrup containing from 20 to 25 per cent. of sugar in a quantity
equal to the capacity of one of the chambers situated on opposite sides of the stone
'the apparatus is then allowed to cool after which the same operations may be
repeated.
The saccharine juices thus obtained are fitted to be subjected to the processes
usually employed in sugar refineries.
The conditions enabling the synthesis of sugar by the combination of the three
bodies, ethylene or other hydrocarbon, carbonic acid and water to be effected as herein-
before described may evidently be obtained without having recourse to the action
of endosmose and the invention may be carried out with the aid of any other suitable
means enabling the aforesaid three elementary bodies to be combined in the proportions
indicated the action of endosmose being in fact only one of the means which may be
employed for carrying out in practice the process of manufacturing sugar by synthesis
according to this invention.
Dated this 20th day of July 1893
J. H. JOHNSON & Co.,
47, Lincoln's Inn Fields, London, W.C., Agents.
COMPLETE SPECIFICATION.
Improvements in the Manufacture of Sugar and in the Apparatus
Employed therein.
I, JAMES YATE JOHNSON of 47 Lincoln's Inn Fields in the County of
Middlesex Gentleman do hereby declare the nature of this invention (which
has been communicated to me from abroad by Jean Ercole Pellegrini of Calle
Cazanova 75 and 77 Barcelona in the Kingdom of Spain Chemist) and in what
manner the same is to be performed to be particularly described and ascertained
in and by the following statement :—
This invention relates to the manufacture of sugar, and enables crystallisable
sugar, (cane sugar), to be produced by synthesis of carbonic acid, ethylene, (or
other suitable hydrocarbon, as hereinafter set forth,) and water; the said synthesis
being performed by osmotic action (or as it is sometimes termed catalysis, or, less
accurately, endosmose) for which purpose it is preferred to employ a specially
constructed apparatus composed of pumice stone prepared, and arranged, as
hereinafter more fully set forth.
The process for the manufacture of crystallisable sugar by synthesis according

page_text: to this invention is based upon the combination of carbonic acid, ethylene, (or other
suitable hydrocarbon as hereinafter set forth,) and water, brought together, under
special conditions, and in the case of ethylene in the proportions indicated by the
formulæ 4 CO, +4 C₂H. + 3 H₂O = C₁₂O₁ representing the typical composition
of crystallisable sugar.
12 22 11
The osmotic action which is the means employed in practice for effecting according
to this invention the synthesis of these three constituents of crystallisable sugar is
by preference employed by means of the specially constructed apparatus which I
now proceed to describe.
This apparatus is shewn in the accompanying drawings.
Figure
of the said drawings illustrates the apparatus in perspective, a part of
the casing being broken away so as to expose the interior.
Figure 2 represents a longitudinal section of a portion of a block of porous
material employed in said apparatus, the central and lower parts being broken away,
which block constitutes the catalytic agent by means of which the synthesis is
accomplished.
Figure 3 represents part of this block in end view.
This apparatus consists of a block of porous material in the form of a cube made
of pumice stone which is a highly porous material and very readily permeated by
gases. In this block are bored numerous deep holes or passages a which do not
pass completely through the block but extend from each side to within say
about 0-8 of an inch from the opposite side. These passages are about one eighth
of an inch in diameter and are parallel with one another.
In order to obtain the best results the blocks are manufactured in the following
manner: Pumice stone is taken, preferably choosing light coloured and heavy
pieces, and it is cleansed by washing it with dilute hydrochloric acid several times,
then with sulphuric acid, and finally with water until the wash water is neutral.
It is then dried thoroughly, and powdered, passed through a fine sieve, and to it is
added ten per cent., by weight, of dry clay, (as free from iron as possible), and
three per cent. of powdered cork both in a like state of division. This mixture is
made into a homogeneous paste with a solution of common salt (specific gravity
about 1120). It is next dried by exposure to air for about 15 days after which it
is placed in a stove heated to about 300° or 400° centigrade. It is allowed to
remain in this stove during 4 or 5 days by which time it is dried throughout and it
is then transferred to a pottery furnace. The furnace should be cold or nearly so
at the time that the material is placed in it and is then suitably heated with a view
to thoroughly baking the material. When this is effected it is damped down the
material being left in it until it is quite cold. The block is then drilled and
afterwards platinized by being immersed in a 10% solution of platinic chloride
(Pt C) or other suitable salt of platinum which will, when sufficiently heated,
deposit finely divided platinum in the pores of the block. This process of
platinization will generally have to be repeated 2 or 3 times before the block is
finished. The boiling in each case is continued for about 3 hours after which the
block is dried in the stove and subsequently heated in a furnace at a cherry red heat,
when, after a few hours exposure, it will be found that the platinum is deposited.
The block should weigh from 1-2 to 1.8 grammes per cubic centimetre before
drilling and if it is homogeneous it will be found that the weight of platinum
deposited by the second boiling will be approximately the same as that deposited
by the first boiling and if such is not the case the block will generally be found to
be non-homogeneous and unsuitable for use.
In order to ascertain that the block after platinization is suitable for the purpose
and not affected by any concealed defects it should be tested by being introduced
into an atmosphere of dry steam and careful observation made as to whether the
steam is decomposed into its constituents oxygen and hydrogen. If such is not
the case it must be platinized once or even twice more until it is capable of
producing that effect.
It is placed, ap
In the figures A represents the block in the form of a cube.

page_text: there shown, in a rectangular box or case D, of cast iron, or other suitable material,
of an internal length 3 times greater than the side of the cube and of a width
and height which are exactly equal to the side of the cube. The block occupies
the middle of this box with the passages a lying in horizontal position and
extending in the direction of the length of the side of the box. It is retained in
position by two steel plates one of which is represented at B and the other at C
perforated with holes registering exactly with the holes in the block so that the
gases, which, as hereinafter explained, are supplied to two chambers A' and A",
on each side of the block A, enter the passages a formed in the said block.
The interior of the case or box is nickel plated, and planed, and is hermetically
closed so as to prevent any leakage of gas. At the ends E and F the case com-
municates with tubes e and f supplying carbonic acid and ethylene respectively.
Each tube is provided with means for regulating the proportions of the gases and
has on it a meter G for measuring the volume-a gauge H for indicating the
pressure and a regulating valve I. The pipe J provided at the upper part of the
apparatus supplies steam through two branches communicating with the upper part
of the chambers A' and A". This pipe is provided with a valvej for regulating
the quantity of steam supplied to the apparatus. The inside of the box or case
likewise communicates with two branch pipes K enabling the chambers A'-A" to
be emptied through a valve k. In working this apparatus the valves k and j are
closed and the valves I are open. Ethylene is then forced under slight pressure
into the compartment A-and carbonic acid is supplied at about the same pressure
to the compartment A". By means of the devices hereinbefore referred to the
supply of the two gases is regulated in such a manner that they pass into the
apparatus in quantities giving equal volumes, at equal pressures and temperatures.
After a few moments the valve j is opened and steam is introduced into the
chambers or compartments A-A" through the pipe J in such manner that the
pressure in the chambers does not rise much. The steam should be dry and at a
pressure of about two, or three, atmospheres in the boiler and may, with advantage,
be somewhat superheated to prevent condensation.
The apparatus becomes rapidly heated. The supply of gases and vapour is
continued during about half an hour but must not be so long continued that the
temperature rises above 150° centigrade and a lower temperature not exceeding
100° centigrade will be found to be more suitable. The gases mix by osmotic action
through the substance of the pumice stone and on the expiration of this period
there is extracted through the discharge valve k a syrup containing from 20% to
25% of sugar the apparatus is then allowed to cool after which the same operations
may be repeated.
It will be understood that the foregoing description of the apparatus and process
is I believe found to be most advantageous to make and carry out, but other forms
of apparatus for producing like osmotic or catalytic action may be used and other
substance, capable of like action, may be substituted for the platinized pumice cube
herein before described.
The regulation of the pressures and temperatures of the gases and vapours
employed may be guided by the consideration that the product should be free from
distinct acid reaction.
I have described the process with regard to ethylene but hydrocarbons of the
olefiant series may replace ethylene if they be such that they are caused to unite by
osmotic action in the requisite proportions with carbonic acid and vapour of water,
acetylene is an example of this kind.
The saccharine juices thus obtained are fitted to be subjected to the processes
usually employed in sugar refineries.
Having now particularly described and ascertained the nature of this said inven-
tion and in what manner the same is to be performed I declare that what I
claim is :-
1. The production of crystallisable sugar by the synthesis of the three bodies,

page_text: namely carbonic acid, ethylene, and water, combined in the proportions indicated by
the formula 4 CO, +4 C,H. + 3 H₂O.
2. The production of crystallisable sugar by the synthesis of ethylene, carbonic
acid, and water, the said synthesis being effected by osmotic, or catalytic, action.
3. The production of crystallisable sugar by the synthesis of any suitable
hydrocarbon of the olefiant series (CnH₂n) with carbonic acid and water.
4. The production of crystallisable sugar by the synthesis of any suitable
hydrocarbon of the olefiant series (CnH₂n) carbonic acid and water the said synthesis
being effected by osmotic or catalytic action.
5. The herein described apparatus for effecting the synthesis of crystallisable
sugar from ethylene or other suitable hydrocarbon of the olefiant series (CnH₂n)
carbonic acid and water by osmotic or catalytic action.
6. The production of crystallisable sugar by synthesis substantially as herein
described.
Dated this 21st day of May 1894.
JOHNSONS & WILLCOX,
47, Lincoln's Inn Fields, London, W.C., Agents.