IMPROVEMENTS IN THE COMBINATION OF CHEMICAL MATERIALS FOR SCOURING, BLEACHING, AND DYEING WOOL, COTTON, SILK, AND OTHER MATERIALS."AL SP
Year: 1860

page_text: LETTERS PATENT to E. Freeman Prentiss, of the City of Philadelphia,
in the United States of America, Manufacturing Chemist, for the Inven-
tion of "IMPROVEMENTS IN THE COMBINATION OF CHEMICAL MATERIALS FOR
SCOURING, BLEACHING, AND DYEING WOOL, COTTON, SILK, AND OTHER
MATERIALS."
PROVISIONAL SPECIFICATION left by the said E. Freeman Prentiss at
the Offico of the Commissioners of Patents, with his Petition, on the
1st November 1860.
I, E. FREEMAN PRENTISS, of the City of Philadelphia, in the United States
of America, Manufacturing Chemist, do hereby declare the nature of the said
Invention for "IMPROVEMENTS IN THE COMBINATION OF CHEMICAL MATERIALS FOR
SCOURING, BLEECHING, AND DYING WOOL, COTTON, SILK, AND OTHER MATERIALS,"
be as follows (that is to say) :-
In the process of scouring and bleaching, in place of using soda ash or
carbonate of soda, as now practised, the Inventor uses a compound formed by
grinding and mixing together 66 parts of soda ash with 48 parts of muriate of
soda, and 9 parts of silacate of soda. Sometimes the relative proportions
herein-before described may be slightly varied to suit particular circum-
stances.
The second part of these improvements consists in the employment of

page_text: sulphate or chloride of manganese in the formation of a "mordant," to be
used in the process of dying, which improved "mordant" is obtained and
prepared as follows:-The sulphate or chloride of manganese (the usual
residuum in making chloride of lime) as it comes from the retorts or stills
used in making chloride of lime, contains as a residuum more or less free acid,
which must be expelled by gently boiling the liquor, or by the use of quick-
lime when the "mordant" is required in its liquid and neutral state. It is to
be used in its liquid and neutral state for browns on cotton, and with metallic
bases for other colours.
To prepare the "mordant" of manganese above spoken of in combination
with other metallic bases, it is requisite to use the acid solution of chloride or
sulphate of manganese as they come fresh from the stills or retorts while still
hot, and then to immerse in this solution the metal required, say, copper, iron,
or zinc.
Iron is to be used when the mordant is desired to give the material
dyed a blue or dark shade of drab, &c. Enough of iron is to be used to entirely
neutralize the acid. Zinc is to be used with iron in the proportion of 8 p
of zinc to the iron when the mordant is desired to be used in the production
of black and blue and some shades of drab. Copper is substituted for iron or
zinc when the colour desired is cutch brown, sufficient copper being used to
neutralize the free acid in the liquor. These metals will be acted upon by the
solutions, and will take up the free acid therefrom and form therewith the
corresponding salts, sulphates, or chlorades, except with copper, according to
the acid contained the heat of the solution will be sufficient generally to effect
the combination. When the acid is thus removed or ceases to act any longer,
the metal is to be withdrawn, and the mixed solutions evaporated to chrystali-
zation.
The above mordants can be used with the ordinary dyes, and in the manner
similar to other known mordants, but to make it more plain for the operator
some of the principal modes of proceeding are given below.
For drab on cotton and wool piece goods, run the pieces to be dyed through
sumac liquor, and then through the manganese in solution; the goods are then
ready to receive any shade of colour desired by the usual way employed for
dying such colours.
To prepare 250 lbs. cotton warps for producing black satinets. Boil the
warps well in clean water, fill up the tub with clean water, so as to cover the
lower rollers about 6 inches, add. 8 lbs. manganese chrystals, previously dissolved
in hot water, run the warp through them, then add 7 lbs. more manganese
dissolved as before, and run the warp through again; save your liquor for
another set of warps, and continue to prepare 250 lbs. more warps in the same

page_text: liquor by adding 12 lbs. more manganese in the same way as in the first
operation; keep the liquor in the tub, and for every 250 lbs. warps add 12 lbs.
more chrystals as before; the warps are now ready for sizing and manu-
facture.
After the satinets are manufactured, cleaned, and fulled, dye them in the
piece with chrome black; if from any circumstance the cotton and wool should
not turn out the same shade of black, top off with a small quantity of blue
vitrol, say, 1 lbs. blue vitrol to 100 lbs. satinets.
For Prussian blue on cotton (100 lbs.) Boil the cotton well in clean water;
then run them through a solution made from 8 lbs. manganese chrystals, and
I lbs. tin chrystals for 10 minutes; then wring out and run them through a
solution of 3 lbs. red prussiate, and 3 lbs. oil of vitrol for 10 minutes, wring
out again, and run them 14 minutes through the first solution, then wring out
and run them 14 minutes through the last solution of red prussiate and oil
of vitrol. Keep the liquor in the tub, and for another 100 lbs. of cotton or yarn,
add 4 lbs. manganese chrystals, and 1 lb. tin chrystals; and to the second tub
add 3 lbs. red prussiate and 1 lb. oil of vitrol, and operate as before. For a
darker shade of blue, top off with logwood and muriate of tin in the proportion
of 1 lb. of logwood to 1 oz. muriate of tin.
For 250 lbs. black cotton warps. Boil the warps well in clean water, fill up
the tub with clean water, so as to cover the lower roller about 6 inches, add
7 lbs. manganese, previously dissolved in hot water, run the warps through.
them, add 5 lbs. more manganese dissolved in the same manner, and run the
warps through again, draw off the liquor meanwhile, and preserve it for
another set of warps; fill up the tub with clean lime water, and run the warps
through, draw off the lime water and fill up with clean lime water, and run
the warps through again, draw off the lime water and fill up with logwood and
bark liquor, previously prepared by boiling 113 lbs. logwood, 30 lbs. quercitron
bark in sufficient water to fill the tub twice; run the warps through this
liquor, then draw off and fill up again with the other part of logwood and
bark liquor, then run the warps through again, add to this liquor 1 lbs. of
blue vitrol previously dissolved in hot water; then run the warps through,
after which add another pound blue vitrol dissolved in hot water, then run the
warps through again. At the second run in the manganese liquor, also at the
second run in the lime water liquor, put extra weight on the rollers so as to
squeeze the warps out as dry as possible. The manganese liquor preserved from
first treatment can now be used for another set of warps of 250 lbs. by adding
9 lbs. manganese dissolved as before; this same manganese liquor can be used
as often as required by adding to it 6 lbs. manganese dissolved as heretofore

page_text: every time it is used. The lime water must be clear and not too strong; it
must have a sweetish and not too pungent taste.
A fast black (which will stand fulling) for 250 lbs. cotton warps. Boil the
warps well in 23 lbs. Sicily sumac and 10 lbs. quercitron bark, after which the
treatment is the same as in the receipt for the black last above described.
A cutch brown for 100 lbs. cotton. Use 4 lbs. of manganese, a liquid in
place of the blue vitrol commonly used; add these to 4 lbs. of catechu, and a
much better colour will be obtained than in the ordinary manner. The second
process is precisely the same as in the ordinary way of dying catechu brown
with soda and bichrome.
Buff for 250 lbs. of cotton warps. Boil the warps well in clean water; then
fill the tub 6 inches above the lower roller, then add 9 lbs. manganese pre-
viously dissolved in warm water, and run the warp through, and then add
4 lbs. more manganese dissolved as before, with a pint of aqua-ammonia fluid,
run the warps through again, add 3 lbs. more manganese and 1 pint of aqua-
animonia, run the warps through again, then draw off the liquor, and preserve
it for another set, which will requiro only 12 lbs. manganese for every
additional set, the treatment is the same as above, only you use 6 lbs. man-
ganese for the first treatment, and 3lbs. for each of the other treatments, with
the same amount of ammonia. After the treatment in the manganese liquor,
and it having been drawn off, fill up the tub with strong lime water, and 'run
the warps through it, and so continue to fill up, and draw off for 3 times
running, the warps once through each liquor, after which the warps are to be
well watered in cold water. For dying cotton or cotton yarn any of the above
colour, the same treatment and quantities will be required.
By using about equal parts of terra japonica and common cutch with about
10 per cent. sulphate or muriate of manganese in sufficient water to dissolve
the terra japonica and cutch when heated by steam or other convenient way,
a better colour is obtained than by using cutch alone, and little or no blue
vitrol will be required to produce the desired colour.
SPECIFICATION in pursuance of the conditions of the Letters Patent, filed
by the said E. Freeman Prentiss in the Great Seal Patent: Office on
the 30th April 1861.
TO ALL TO WHOM THESE PRESENTS SHALL COME, I, E. FREEMAN
PRENTISS, of the City of Philadelphia, in the United States of America, 3
Manufacturing Chemist, send greeting.

page_text: WHEREAS Her most Excellent Majesty Queen Victoria, by Her. Letters
Patent, bearing date the First day of November, in the year of our Lord
One thousand eight hundred and sixty, in the twenty-third year of Her reign,
did, for Herself, Her heirs and successors, give and grant unto me, the said
E. Freeman Prentiss, Her special licence that I, the said E. Freeman Prentiss,
my executors, administrators, and assigns, or such others as I, the said E.
Freeman Prentiss, my executors, administrators, and assigns, should at any
time agree with, and. no, others, from time to time and at all times there-
after during tho 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 "IMPROVE-
MENTS IN THE COMBINATION OF CHEMICAL MATERIALS FOR SCOURING, BLEECHING,
AND DYING WOOL, COTTON, SILK, AND OTHER MATERIALS," upon the condition
(amongst others) that I, the said E. Freeman Prentiss, my executors or
administrators, by an instrument in writing under my, or their, or one.
of their hands and seals, should particularly describe and ascertain the
naturo 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 1, the said E. Freeman Prentiss, do hereby declaro
the nature of my said Invention, and in what manner the same is to be per-
formed, to be particularly described and ascertained in and by the following
statement, that is to say:-
In the process of scouring and bleaching in place of using soda ash or
carbonate of soda, as now practised, I use a compound formed by grinding
and mixing together 66 parts of soda ash with 48 parts of muriate of soda,
and 9 parts of silicate of soda. But sometimes the relative proportions
before described may be slightly varied to suit particular circumstances.
The second part of these my said improvements, consists in the employment
of sulphate or chloride of manganese in the formation of a "mordant" to be
used in the process of dying, which improved "mordant" I obtain and
prepare as follows:-The sulphate or chloride of manganese (the usual
residuum in making chloride of lime) as it comes from the retorts or stills
used in making chloride of lime contains as a residuum more or less free acid,
which must be expelled by gently boiling the liquor, or. by the use of quick-
line, when the "mordant" is required in its liquid and nentral state.
it in its liquid and neutral state for browns on cotton, and with metallic bases
for other colours.
I usc

page_text: To prepare the "mordant" of manganese above spoken of in combination
with other metallic bases. I use the acid solutions of chloride, or sulphate of
manganese, as they come fresh from the stills or retorts while still hot, and
then immerse in the solution the metal required, say copper, iron, or zinc.
Iron is used when the "mordant" is desired to give the material dyed a blue
or dark shade of drab. Enough of iron is used to entirely neutralize the acid.
I use zinc with iron in the proportion of 8 per cent. of zinc to the iron when
the "mordant" is desired to be used in the production of blacks and blues,
and some shades of drab. I substitute copper for iron or zinc when the
colour desired is cutch brown, sufficient copper being used to neutralize the
free acid in the liquor. These metals will be acted upon by the solutions, and
will take up the free acid therefrom and form therewith] the corresponding
salts, sulphates, or chlorides (except with copper) according to the acid con-
tained, the heat of the solution will be sufficient generally to effect the
combination, when the acid is thus removed or ceases to act any longer,
the metal is withdrawn, and the mixed solutions evaporated to crystallization.
The above "mordants" can be used with the ordinary dyes, and in the
manner similar to other known "mordants," but to make it more plain
for the operator, some of the principal modes of proceeding are given
below.
For drying a drab on cotton, and wool piece goods, I run the pieces to be
dyed through sumac liquor, and then through the manganese in solution. The
goods are then ready to receive any shade of colour desired in the usual way
employed for dying such colours.
To prepare 250lbs. of cotton warps for producing black satinets. I boil the
warps well in clean water, and fill up the tub with clean water, so as to cover
the lower rollers about 6 inches and add Slbs. manganese crystals, previously
dissolved in hot water, I run the warps through, and then add 7lbs. more manga-
nese dissolved as before, and run the warps through again. I save the liquor for
another set of warps, and continue to prepare 250lbs. more warps in the same
liquor by adding 12lbs. more manganese, in the same way as in the first
operation. I keep the liquor in the tub, and for every 250lbs. warps add 12lbs.
more crystals as before, the warps are now ready for sizing and manufacture.
After the satinets are manufactured, cleaned, and fulled, I dye them in the
piece with chrome black. If from any circumstance the cotton and wool should
not turn out the same shade of black I top off with a small quantity of blue
vitrol say 1lbs. blue vitrol to 100lbs. satinets.
For prussian blue on cotton (100lbs.,) I boil the cotton well in clean water
then run them through a solution made from 8lbs. of manganese crystals, and

page_text: 1lb. tin crystals, for 10 minutes, then wring out and run them through a
solution of 3lbs. red prussiate, and 3lbs. oil of vitrol, for 10 minutes, I
wring out again, and run them for about 14 minutes through the first
solution, then wring out, and run them about 14 minutes through the last
solution of red prussiate and oil of vitrol. I keep the liquor in the tub, and
for another 100lbs. of cotton or yarn add 4lbs. manganese crystals, and 1lb.
tin crystals, and to the second tub, I add 3lbs. red prussiate and 1lb. oil of
vitrol, and operate as before. For a darker shade of blue, I top off with log
wood and muriate of tin in the proportion of 1lb. of logwood to loz. of muriate
of tin.
For 250lbs. black cotton warps. I boil the warps well in clean water, fill up
the tub with clean water, so as to cover the lower rollers about 6 inches, and
add 7lbs. manganese previously dissolved in hot water, I run the warps through
and add 5lbs. more manganese dissolved in the same manner, and run the
warps through again. I draw off the liquor meanwhile and preserve it for
another set of warps. I fill up the tub with clean lime water, and run
the warps through, then draw off the lime water, and fill up again
with clean lime water, and run the warps through. I draw off the lime water
and fill up with logwood and bark liquor previously prepared by boiling 113lbs.
logwood and 30lbs. quercitron bark in sufficient water to fill the tub twice. I
run the warps through this liquor, then draw off and fill it up again with the
other part of logwood and bark liquor, then run the warps through again. I
add to this liquor lbs. blue vitrol previously dissolved in hot water,
then run the warps through it after which I add another pound blue vitrol
dissolved in hot water, then run the warps through again. At the
second run in the manganese liquor, also at the second run in the lime water
liquor, I put extra weight on the rollers, so as to squeeze the warps out as dry
as possible. The manganese liquor preserved from the first treatment can now
be used for another set of warps of 250lbs. by adding 9lbs. of manganese
dissolved as before, the same manganese liquor can be used as often as
required, by adding to it 6lbs. manganese dissolved as heretofore every time it
is used. The lime water must be clear and not too strong, it must have a
sweetish and not too pungent taste.
A fast black (which will stand fulling) for 250lbs. cotton warps. I boil the
warps well in a solution containing 23lbs. Sicily sumac, and 10lbs. quercitron
bark after which the treatment is the same as in the receipt for the black, last
above described..
A cutch brown for 100lbs. cotton. I use 4lbs. manganese liquid in place of

page_text: the blue vitrol commonly used, and add this to 4lbs. of catechu, and a much
better colour is obtained than in the ordinary manner. The second process is
precisely the same as in the ordinary way of dying catechu brown with soda
and bichrome.
Buff for 250lbs. of cotton warps. I boil the warps well in clean water, then
fill the tub 6 inches above the lower rollers, then add 9lbs. manganese
previously dissolved in warm water, and run the warps through it, and then
add 4lbs. more manganese, dissolved as before, with a pint of aqua ammonia
fluid. I run the warps through again, add 3lbs. more manganese and 1 pint
of aqua ammonia, and run the warps through again, then I draw off the
liquor and preserve it for another set which will require only 12lbs. manganese
for every additional set, the treatment is the same as above, only I use 6lbs.
manganese for the first treatment, and 3lbs. for each of the other treatments
with the same amount of ammonia. After the treatment in the manganese
liquor, and it having been drawn off, fill up the tub with strong lime water, and
run the warps through it, and so continue to fill up and draw off for 3 times,
running the warps once through cach liquor, after which the warps are to be
well washed in cold water.
For dying cotton or cotton yarn any of the above colours, the same treatment
and quantities will be required. By using about equal parts of terra japonica
and common cutch with about 10 per cent. of sulphate or muriate of manga-
nese in sufficient water to dissolve the terra japonica and cutch when heated
by steam or other convenient way, a better colour is obtained than by using
cutch alone, and little or no blue vitrol will be required to produce the desired
colour.
The advantage of this my improved "mordant" is its economy, as it utilizes
what would otherwise be a waste material or residue in the manufacture of
chloride of lime, its efficiency as a "mordant" for dying mixed cotton and
wool piece goods, as it acts equally, effectually on both the cotton and wool,
which is a desideratum.
Having now fully described and ascertained the nature of these my said
improvements, and how I believe the same may be best put to practical use,
I wish it to be understood that I do not confine myself to the preciso details
or relative proportions, as it will be readily seen by all acquainted with the art
that they may be varied without departing from my Invention, at the same
time I do not claim the use of chloride or sulphate of manganese and iron as a
dye; but what I do claim as new and my Invention is,―
First, the chemical manufacture of the compound herein-before described

page_text: and the application thereof to the scouring and bleaching of cotton, silk,
and other materials, substantially and in the manner herein-before described
and set forth.
And lastly, the use of chloride of manganese and iron, or a sulphate of
manganese and iron, prepared substantially and in the manner herein-
before described and set forth, as a "mordant" to be used with the
ordinary dyes.
In witness whereof, I, the said E. Freeman Prentiss, have hereunto set
my hand and affixed my seal, this Twenty-ninth day of April, in the
year of our Lord One thousand eight hundred and sixty-one.
Witness,
WILLIAM WALKER,
of 44, Castle Street,
Liverpool.
E. FREEMAN (L.S.) PRENTISS.