IMPROVEMENTS IN THE MANUFACTURE OF WOOLLEN AND SILKEN FABRICS, AND OF SOAP AND DETERGENTS FOR USE IN THESE MANUFACTURES, AND FOR OTHER PURPOSES." PROVISIONAL SPECIFICATION
Year: 1875

page_text: LETTERS PATENT to John Thomas Way, of No. 9, Russell Road,
Kensington, in the County of Middlesex, for the Invention of
"IMPROVEMENTS IN THE MANUFACTURE OF WOOLLEN AND SILKEN FABRICS,
AND OF SOAP AND DETERGENTS FOR USE IN THESE MANUFACTURES, AND FOR
OTHER PURPOSES."
PROVISIONAL SPECIFICATION left by the said John Thomas Way at
the Office of the Commissioners of Patents, with his Petition, on
the 8th November 1875.
•
I, JOHN THOMAS WAY, of No. 9, Russell Road, Kensington, in the
County of Middlesex, do hereby declare the nature of the said Invention
for "IMPROVEMENTS IN THE MANUFACTURE OF WOOLLEN AND SILKEN FABRICS, AND
OF SOAP AND DETERGENTS FOR USE IN THESE MANUFACTURES, AND FOR OTHER
PURPOSES," to be as follows:-
This Invention has for its object improvements in the manufacture of

page_text: woollen and silken fabrics, and of soap and detergents for use in these
manufactures, and for other purposes.
I have found that compounds in which phosphoric acid is combined
with alumina and soda or potash in the proportion of single equivalents
of the two former substances to three or to four equivalents of the
alkali respectively have valuable detergent properties. To these
compounds or double salts the empirical formulæ may be given :-
compounds or double salts the empirical formulæ may be given
Na O Al, 0, + 2 Na O Ho P₂ О, + Aq, and
2
2
Na O Al, 0, +3 Na-O P, 0, + Aq.
5
When any fatty or greasy or analogous substance is brought in
contact with solutions of these salts the alkali is given up, whilst at the
same time the alumina combines with the phosphoric acid as phosphate
of alumina. In these salts a larger proportion of the alkali is therefore
available for detergent purposes than in the triphosphate of soda which
is the subject of former Patents granted to me.
In describing the processes to which I resort I shall refer to the
alkali soda only, but I wish it to be understood that with proper
modifications of the proportions potash is equally applicable.
To a saturated solution of alumina in soda, or to aluminate of soda,
I add ordinary or rhombic phosphate of soda until the mixture, when
tested with nitrate of silver, no longer produces a brown or black
precipitate. I evaporate the solution so obtained till it becomes thick,
and allow it to cool when, if the evaporation has been carried sufficiently
far, I obtain a soft saline material.
I produce a similar compound, though not in the same proportions,
by dissolving hydrated alumina in triphosphate of soda by the aid of
heat. Or I dissolve phosphate of alumina, whether natural or artificially
produced, in solution of caustic soda; or I heat the phosphate of
alumina with caustic soda or carbonate of soda, or both, in a furnace.
In either case a soluble compound of phosphoric acid, alumina, and
soda is produced which may be separated from sand and other insoluble
matters by subsidence or filtration, and obtained in the solid form by
evaporation, as before described.
If I require to produce the salt in a white state it is necessary to
calcine the native phosphate of alumina before dissolving it in solution
of caustic soda.

page_text: The proportions of caustic or carbonate of soda should be so arranged
that for every equivalent of phosphoric acid there should be not less than
three and not more than four equivalents of soda.
Caustic Of Carbonate of sou should be so arranged
that for every equivalent of phosphoric acid there should be not less than
three and not more than four equivalents of soda.
The salt obtained by either of these processes I employ in the
manufacture of wool and silk.
In the manufacture of wool I employ it in the various scourings to
which the fibre or fabric is submitted in the process of manufacture in
lieu of soap or other detergent.
In the manufacture of silk I employ the salt to remove the natural
gum from the fibre.
In the preparation of soap I add to soap in the melted condition any
desired proportion of the compound or compounds before described;
having first melted this also by the application of a gentle heat I stir
the materials together until proper admixture has been obtained, and
allow the compound soap to cool in frames in the usual way.
In some cases I use the compound in the actual saponification of
fatty matters I proceed as follows:-I heat the grease or oil with a
strong solution of caustic soda, in which the quantity of alkali iš,
somewhat short of that which is necessary for the complete saponification
of the fatty matters; after a time I add the compound of phosphoric
acid, alumina, and soda; and continue to heat until the whole of the
grease is converted into soap; or I obtain the same result by mixing the
whole of the materials at the beginning of the operation:
I propose to employ the product of this process as soap without
separation of niger or lye, as usually practised.
:
The triphosphates of soda may be used in the same manner in the
production of soap, or the rhombic phosphate of soda may be employed.
In this latter case I prefer to saponify the grease with the quantity of
alkali which is known to be necessary and an additional quantity,
sufficient to convert the diphosphate of soda which it is proposed to use
into triphosphate. The diphosphate or rhombic phosphate of soda is
melted and added to the other materials: when the saponification is

page_text: In some cases I employ the salts of phosphoric acid, alumina, and
soda in conjunction with silicate of soda or sulphate of soda, or both.
I can also use the salts in any desired proportion with triphosphate of
anda
SPECIFICATION in pursuance of the conditions of the Letters Patent
filed by the said John Thomas Way in the Great Seal Patent
Office on the 8th May 1876.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, JOHN
THOMAS WAY, of No. 9, Russell Road, Kensington, in the County of.
Middlesex, send greeting.
WHEREAS Her most Excellent Majesty Queen Victoria, by Her
Letters Patent, bearing date the Eighth day of November, in the
year of our Lord One thousand eight hundred and seventy-five, in the
thirty-ninth year of Her reign, did, for Herself, Her heirs and
successors, give and grant unto me, the said John Thomas Way, :
Her special license, that I, the said John Thomas Way, my exe-
cutors, administrators, and assigns, or such others as I, the said
John Thomas Way, my 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 THE MANUFACTURE OF WOOLLEN AND SILKEN
FABRICS, AND OF SOAP AND DETERGENTS FOR USE IN THESE MANUFACTURES, AND
FOR OTHER PURPOSES," upon the condition (amongst others) that I, the
said John Thomas Way, my executors or administrators, by an instru-
ment in writing under my, or their, or one of their hands and seals,
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 immediately after the date of the said Letters
Patent.
NOW KNOW YE, that I, the said John Thomas Way, do hereby

page_text: to be particularly, described and ascevante in anu
by the following statement thereof, that is to say :-
This Invention has for its object improvements in the manufacture of
woollen and silken fabrics, and of soap and detergents for use in these
manufactures, and for other purposes.
I have found that compounds in which phosphoric acid is combined
with alumina and soda or potash in the proportion of single equivalents
of the two former substances to three or to four equivalents of the
alkali respectively have valuable detergent propertics. To these com-
pounds or double salts the empirical formulæ may be given:-

page_text: provided that sufficient phosphate of soda be employed to counteract
causticity, as before explained..
2
I produce another form of salt by dissolving alumina in solution of
triphosphate of soda (3 Na O P. O,), by the aid of heat. The solution
of phosphate of soda may be of any convenient strength, say 1 part of
crystallized phosphate in 3 or 4 parts water; it is brought to the boiling
point and the alumina added by degrees, the heat being kept up till the
alumina ceases to dissolve. The solution is filtered and evaporated as in
the last case.
A solution containing one hundred parts of trisodic
phosphate will dissolve from 6 to 7 parts of alumina.
When treating native phosphate of alumina with caustic soda I
proceed as follows:-Having ascertained by chemical analysis the pro-
portion of phosphoric acid contained in the mineral phosphate, I
calculate the quantity of commercial caustic soda which it will be
necessary to use to any convenient quantity of the said mineral, so that
for every 71 parts of phosphoric acid there may be from 93 to 109 parts
of real soda (Na O), these numbers being in the relation of 1 equivalent
of phosphoric acid to 3 or 3 equivalents of soda. I dissolve the
caustic soda in from 10 to 15 times its weight of water by heat, and.
when this solution is at the boiling point I add by degrees the phosphate
of alumina previously reduced to powder; after all the mineral has been
added I continue the boiling for half an hour or an hour in order that
the coarser particles of rock may be dissolved. I now filter a portion of
the liquor and test a few drops by a neutral solution of nitrate of silver;
if a strong brown tint is exhibited there is an excess of caustic soda
present in this case I add small successive quantities of powdered
mineral, boiling up the liquor meanwhile and testing after each addition
until little or no brown color is produced by the tests; if the liquor
after the first boiling should be found to be free from causticity small
quantities of caustic soda in solution must be added until it just indicates
the presence of free caustic alkali. I allow the liquor to rest for a few
hours, when the greater part can be decanted off nearly clear, and is
further cleared by filtration. I wash the insoluble residue, using the
wash waters for further operations, as is well understood, the liquor so
made should have when cold a specific gravity of about 1·100
(20° Twaddell). I boil this liquor down rapidly in iron vessels (by
preference galvanized iron) until it marks at the boiling temperaturę
from 65° to 70° Twaddell (1-325 to 1.350, specific gravity), I then
་་

page_text: remove the concentrated liquor as quickly as possible from the evapo-
rating pan and cool it by running it out on to a clean cold floor or in
shallow pans dipping into cold water. The product is a solid saline
body which if properly made should be almost or entirely soluble in
water, and which should melt into a clear transparent liquor. at a
temperature of 150° Fahrenheit or lower.
If necessary I remove any slight causticity by the addition of a small
quantity of rhombic phosphate of. soda to the evaporated salt immediately
before removing it from the pan, the rhombic phosphate may be added
in the crystalline form; it will melt in the hot liquor and be readily
mixed by stirring; rosin or grease will serve the same purpose, and these
may be added at any period of the boiling down.
It is important that the liquor before evaporation should neither
contain a great excess of caustic or an excess of phophate, otherwise it
is liable to decompose during the evaporation. It is also important on
the same ground that the salt should be rapidly cooled. This decom-
position when it occurs is attended with the production of a quantity of
an insoluble white salt, the liquor becomes thick and pasty and cannot
be carried down to the required gravity; the product so altered is in
fact unfit for the purpose to which it is intended to apply it. :. When
notwithstanding the precautions, indicated above this decomposition is
found to occur I return the whole of the material to the boiling pan and
add water and a quantity of caustic soda equal to about or of that
already present in it. I boil the mixture until the white salt is
deposited and then add a quantity of phosphate of alumina equal to the
additional soda that has been employed, after boiling I filter and
evaporate as before. I find that on this second operation there is less
liability of the decomposition of the salt.
The native phosphate of alumina varies much in composition, being
generally mixed with a large proportion of phosphate of iron. The pro-
portion of alkali to be employed will therefore be subject to modifi-
cation, but I will give an instance of the quantities to be used in the
case of a cargo of phosphate of alumina from the Island of Redonda.
This phosphate contains in 100 parts water of combination and organic
matter 21; phosphoric acid 37%; oxide of iron 12; alumina 20;
sand &c., 10. 100 lbs. of this phosphate will require for solution from
about 48 to 56 lbs. of real soda (Na O), or about 70 to 80lbs. of
commercial caustic soda of 70 per cent.
ند.

page_text: I should observe that when the solution of aluminous phosphate in
soda ceases to indicate causticity by nitrate of silver it is still capable of
dissolving a large additional quantity of the mineral, and I sometimes
make solutions in this way, that is to say, by boiling the caustic soda
with an excess of the native phosphate of alumina, but in this case the
liquor requires to be evaporated at a low temperature, say 160° to
180° Fahrenheit, which is best done by means of a vacuum pan.
The native phosphate of alumina when treated as described gives a
salt more or less colored. In order to get a salt of a light color I calcine
the rock in a furnace or kiln. The quantity employed in making the
salt must then be modified in proportion to the loss of weight in the
burning.
I also sometimes decolorize the salt by chlorine or other agent; this
can conveniently be done by adding to the boiling caustic soda solution
(before putting in the mineral) a quantity of bleaching powder equal to
from 7 to 10 per cent. on the mineral to be used.
In making the salt by furnacing phosphate of alumina with carbonate
of soda the following proportions may be taken:-Of raw ground
Redonda phosphate (of the analysis before given) 100 parts; soda ash
of 50 per cent., 97 parts. The mineral and soda ash should be intimately
mixed and furnaced at a low red heat for 2 or 3 hours. The product
should be allowed to cool, and be then dissolved by boiling for an hour
or two in water, and the solution boiled down to the necessary gravity,
as before described. This solution cannot be caustic, neither is it so
liable to, decomposition as when made from caustic soda; for these
reasons the dry process is to be preferred, but it gives a salt containing
a smaller proportion of alumina.
..

page_text: In using any of the compounds made as now described for washing
wool or woollen goods or cleaning silk I-find a solution at the rate of 1
part of the salt to 100 parts of water to be well suited. The solution
may be made either with hot or cold water, and it may be employed with
or without soap. Where the salt is to be used with water containing
much lime or magnesia it is desirable to allow the precipitate of earthy
phosphates which occurs when the salt is dissolved in such water to:

page_text: The triphosphate of soda may be used in the same manner in the
production of soap, or the rhombic phosphate of soda may be employed.
In this latter case I prefer to saponify the grease with the quantity of
alkali which is known to be necessary; and an additional quantity suffi-
cient to convert the diphosphate of soda which it is proposed to use into
triphosphate. The diphosphate or rhombic phosphate of soda is
melted and added to the other materials when the saponification is
complete.

page_text: Seventh. The combination with soap of triphosphate and diphosphate
of soda.
In witness whereof, I, the said John Thomas Way, have hereunto
set my hand and seal, this Fifth day of. May, in the year of our
Lord One thousand eight hundred and seventy-six.
J. THOMAS WAY. (L.S.)