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Патент USA US2412535

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Patented Dec. ‘10, 1946
2,412,535
, UNITED STATES PATENT ‘OFFICE’
1
2,412,535
’
an'rrrnasrmam mamas-non
Earl Leroy Richardson, Bound Brook, and
Kenneth Lyman Russell, Nutley, N. J., assign‘ors
to Colgate-Palmolive-Peet Company, Jersey
City, N. J ., a corporation of Delaware
No Drawing. Application November 29, ‘1944,
Serial No.v 565,810
‘
6 Claims. (Cl. 167-90)
1 f
'
The present invention relates to‘ improved
preparations for retarding or inhibitingv perspira
tion.
2
antl-perspirant agent on fabrics, but also is itself
an anti-perspirant agent.
.
It is an object of this invention, therefore, to‘
'
Certain chemical compounds have the property
‘of retarding, eliminating or inhibiting the flow
provide preparations which inhibit or retard per
spiration and which do not have a corrosive ef
of perspiration, and vmany of them are now.
fect on fabrics.
'
_
widely employed in preparations for that purpose.
Of these compounds, the most commonly used
v preparations which possess the full perspiration
are aluminum salts, such as aluminumv chloride,
retarding effect of the agents incorporated there
It is another object of this invention to provide
aluminum sulphate, and the like, but other com
pounds, such as zinc, iron, tin and bismuth salts,
in for that purpose, and which do not exhibit un
desirable corrosive effect on fabrics.
have also been proposed for the same purpose.
Other objects will be apparent from the dis
Such compounds are termed anti-perspirant
closures herein.
compounds or agents.
7
.
.
The objects of this invention are achieved by
An undesirable consequence of the use of anti 15 providing preparations suitable for use as per
perspirant compounds to stop the flow of pere
spiration-inhibiting or retarding compositions,
spiration has been found to be the corrosive ef
containing aluminum salts now recognized as
possessing that property, and also containing cer
- fect of the composition on clothing. When a
preparation containing these agents is applied to ‘
tain salts of acids of phosphorus which have the
that area of the skin where retarding of the-per 20 effect of reducing or eliminating the corrosive ef
spiration is desired, a portion» of the preparation ' fect of the perspiration-retarding agents upon
may come into contact with and adhere to the
These preparations may contain, as
, fabrics.
agents for inhibiting, retarding or eliminating
clothing of the user. If the garment is ironed,
perspiration in localized areas of the skin to
pressed or otherwise heat-treated before the anti- '
perspirant agent is removed by laundering or 25 which they are applied, water-soluble astringent
‘salts of aluminum. The aluminum salts found
_ cleaning, the corrosive effect of the composition '
is immediately manifested by a reduction in the
strength of that portion of the garment withv
which it has come into contact, sometimes even‘
resulting in holes, that is, a complete 100% de 80
terioration of the garment in speci?c areas. Long
continued contact of the anti-perspirant agent
with a garment, even at ordinary temperatures,
may cause deterioration or reduction in strength .
of the garment. The corrosive action of perspira
tion-retarding compounds is particularly notice
able on fabrics containing cellulosic materials,
‘such as cotton, rayon, and other synthetic ?bers;
however, it is not limited thereto, and may be Obi»?
served on other types of fabrics.
most suitable for this purpose are aluminum sul
phate and aluminum chloride, but other alumi
num salts recognized by the art will serve the
same purpose.
The salts which have the effect of inhibiting or
preventing the corrosive action or the anti-per
spirant agents on fabrics are neutralized salts of
acids of phosphorus, which are stable in solution,
35 asv illustrated by tertiary orthophosphates. Meta
phosphates are not’suitable since'they are not
stable in solution but gradually hydrolyze to form
primary orthophosphates; and the primary and
secondary orthophosphates, the so-called acid
40 salts, are not suitable to achieve the purposes de
sired.
Y
Many methods have been proposed to reduce
this undesirable effect of the perspiration-re
The inhibiting salt may be selected to serve also
as additional anti-perspirant agent in prepara
tarding agents on fabrics, including the incor
poration in the preparation containing the anti
tions in which it is used. In such preparations,
perspirant agent of such addition agents as urea 45 the cation of the inhibiting salt should be alumi
num ion or the cation of some other perspiration
and other amides, and oxides, hydroxides and
inhibiting agent. A highly desirable preparation
carbonates of aluminum, magnesium and zinc,
and other compounds. Some of these addition
may contain aluminum sulphate or chloride and
agents do reduce or neutralize the corrosive ef
aluminum orthophosphate or aluminum pyro
fect of the anti-perspirant compound, but some 50 phosphate. In the making of these preparations
of them also reduce the amount of anti-perspir
or compositions, the aluminum phosphates are
ant agent which has been incorporated in the
added as such.
preparation for thepurpose of retarding per
If an increase in anti-perspirant agent is not
spiration. No compound has yet been proposed
desired, the inhibiting compounds may be pro
which not only reduces the corrosive effect of the
duced in situ. If it is desired to produce these
2,419,585
4
compounds in situ, that is, admixed with the anti
perspirant agent, a suitable soluble'salt of an acid
of phosphorus is added'to a solution containing
_
.
salt to one mol of thevinhibiting agent, or even
less.
sodium pyrophosphate or trisodium orthophos
phate may be added to‘ a solution of aluminum
sulphate, which results in the formation of
It is appreciated that the cosmetic formulator
cannot determine all the usesto which his Prep
arations are to be directed. However, the fore
going instructions will enable the manufacturer
to select the proportion most suitable to his prod
aluminum pyro- ' or orthophosphate.
uct and, in cases of doubt, to include a safe pro- '
the anti-perspirant agent. For'example, tetra
Likewise,
the corrosive effect of the anti-rperspirant com
portion of the ‘corrosion-inhibiting compound.
It appears that aluminum phosphate in solu
tion is itself an anti-perspirant agent, and that.
when added as such (that is, not formed by the
These novel‘ compositions may be made as
reaction of the anti-perspirant compound with
emulsions, solutions, creams, salves, and the like.
a suitable soluble phosphate), it increases the
and may contain any other ingredients which do
not effect a chemical change in the perspiration ~15 potential anti-perspirant action of the prepara
tion.
inhibiting agent or in the fabric-protecting com
The maximum proportion of the protective
pounds and which are not irritating or otherwise
aluminum phosphate that may be used is depend- ‘
unsuited for such preparations. That is, the nov
ent upon the type of preparation to be made;
el preparations may contain common cosmetic
ingredients, coloring bodies, perfumes, and the 20 there is, in fact, no maximum within practical
limits. If a clear anti-perspirant solution is de
like.
i
_
sired, the maximum quantity of the corrosion-in
The usual methods of compounding these prep
hibiting aluminum phosphate'which may be in
arations, such as are suitable for the preparation
corporated therein, that is, in the aluminum sul
of emulsions, solutions, extracts, selves, and the
phate or aluminum chloride solution, is the great
like, may be employed.
est quantity of phosphate which may be dissolved
The proportion of the anti-perspirant agent to
in the solution. (Aluminum orthophosphate is
the total composition may be widely varied and
soluble only to a negligible degree in water, but
is in?uenced by the type of preparation, the fre
it readily dissolves to a considerable degree in a
quency of use, and other like factors, but is gen
erally a matter of choice. As has been disclosed 80 solution of aluminum sulphate.)
In creams, emulsions and other non-transpar
in the prior art, any proportion within the range
ent preparations, the quantity of aluminum phos
of 10% to 30% of hydrated aluminum sulphate
phate may exceed that which will dissolve, par
" makes a satisfactory preparation. In general,
ticularly when the excess phosphate has no un
the same proportions of aluminum chloride have
desirable influence on the stability, appearance,
been found suitable.
or other characteristics of the preparation.
,
The proportion of phosphate salt to the anti
When the inhibiting compound is formed' in
perspirant agent‘ is dictated by the requirements
situ, as by the addition of sodium or potassium
or uses of the preparation. In those cases where
orthophosphate or pyrophosphate to a solution
garments which have come into contact with the
of aluminum sulphate, the effect, if any, of the
preparation are heat-pressed, or otherwise sub 40 by-product‘
sodium or potassium sulphate on the
jected to high temperatures, without first being
preparation should be considered. If this by
laundered, a greater proportion of the corrosion
product salt is undesirable for any reason in the
inhibiting compound is required than otherwise,
preparation, the inhibiting compound should not
-a proportion of two to three mols of aluminum
be formed in situ.
45
orthophosphate to one moi of aluminum sulphate
_Thus, it will be seen that the limits of the
being necessary for complete or substantially
proportions of the aluminum phosphate corro
complete protectionfrom corrosion. It will be
sion-inhibiting compound may vary over a wide
understood that even in those instances the tem
range, and may be any desirable proportion that
perature of the iron or pressing device has a di
reduce or eliminate the corrosive action of
rect relationship to the inhibiting power of the 50 will
the anti-perspirant agent as a minimum and will
phosphate salt. For example, when the tempera
dissolve or not undesirably affect the preparation
position may ‘be inhibited .by using tricalcium or 10
trimagnesium. orthophosphate.
ture of the iron is no more than 250° to 275° F.,
two mols of aluminum orthophosphate to one mol
-
as a maximum.
.In order to determine the corrosive effect, if
of aluminum sulphate will afford substantially
any, of the novel preparations on fabrics, certain
complete protection from corrosion. However, 55 solutions
and preparations were compounded. ap
another factor to be- considered is the length of
plied to fabrics, and the effect thereof upon the
time during which the area containing the anti
tensile strength of the fabric determined.
perspirant agent is subjected to the ironing proc
, In testing anti-perspirant creams, 21/2 grams
ess. For the average time of ironing or pressing
of the. preparation were applied evenly along a
at 250° to 275° F., i. e., ?ve to ten seconds, the
one-inch wide band, in the direction of the ?ll
proportion speci?ed of two mols of aluminum or
ing threads, in the center of a desized cotton
thophosphate to one mol of aluminum sulphate
muslin strip 24 inches long (in the direction of
is satisfactory. Should the garment be such that
the ?lling threads) and 6 inches wide (in the
a higher temperature and/or a longer period of 65 direction of the warp‘ threads) . 'The treated fab- ’
pressing is required, the proportion should be
ric was incubated at about 80° F. and 85-90%
higher.
relative humidity for twenty-four hours. The
In view of the general method of laundering
entire strip was then pressed for ?ve seconds
and ironing garments, in which the cleaning .
with the cream side down against the pad of a
process removes the anti-perspirant agent or sub 70 G. E. flat bed ironer. The temperature of the
stantially all of it, a smaller proportion of alumi
ironer, which had been calibrated, was 293-305‘
num orthophosphate or pyrophosphate to the
F. The ends of the strip were reversed, and the
anti-perspirant agent is satisfactory. Prepara
fabric was again pressed for ?ve seconds. The
tions to be used under conditions of careful laun
test fabric was then returned to the humidity
dering may contain one mol of the phosphate 75 chamber and reconditioned for three hours. after
.
.
8,418,585
6
5
which time it was broken in the warp direction
in a tensile strength testing machine by the
4" x 6" grab method, as outlined by A. S. T. M.
Example V
Parts
Al2(SO4)a.18H-.~O ______________________ __ 25
(American Society for Testing Materials), Desig
AIPO; _'_______________________ -__ ______ __
nation D39-39. As a control, a similar piece of
3.25
H20 ________________ __. ________________ __ 45.75
- the same cotton fabric (with no cream applied)
Tensile strength loss of 54%.
was treated in the same way along with the test
strip. The diil'erence between the average tensile
-
Example VI
strength of the control and test pieces was the .
'
>
Parts
loss (or gain) in tensile strength due to the ef 10 A 34% solution of A1013 _________________ __ 22.4
fect oi’ the cream on the fabric.
In’the case of anti-perspirant solutions, the
muslin strip was folded along its width, and the
folded edge was ‘immersed in the anti-perspirant
H2O ___________________________________ __ 52.6
Tensile strength loss of ‘72.6%.
Example VI‘I
_
solution until there was a one-inch band of so
AlPO4 _______________ __' _______________ _____ 14.0
Tensile strength loss of 34%.
The following examples are formulae of prep
arations which serve to illustrate the invention,
Example VIII
7
NaaPO4J2I-IaO ___________________________ __.. 10
ples of this invention may contain the following 25
ingredients and percentages:
mo
,
_
________ __
Tensile strength loss of 1.7%.
40
'
Example IX
Example I
.
Parts
A12(SO4)3.18H2O ___;___'_ _________________ __ 25
and are not limiting in any sense thereon.
- A suitable preparation embodying the princi
Part I:
Parts
H20 __________________________ __,_-__'____- 38.6 -
20
.
.
A 34% solution of A101: ____________ __'_____ 22.4
lution along the center of the fabric. The ex
cess solution was gently squeezed out, and the
fabric was‘ allowed to hang, _to dry partially, for
?ve minutes. It was immediately pressed under
the same conditions as outlined for creams.
.
Y
.
1'
Parts
vAcid stabilized glycerol monostearate-___ 16
Spermaceti wax ______________________ __
30
5
-Part II:
H2O --__
_
Parts
A1:|(S(__)4)3.18H20 _________ __. ______________ __ 25
Ca:(P04)z'_
‘
4
'
46
Tensile strength loss of 22% .
A12(SO4)3.18H2O _____________________ _- 19
A1PO4 ______________________________ __
Example X
7
Water ____________________________ __'__ 53
'
,
Parts
A12(SO4):I.18H2O __________ __. ___________ __ 25,
The cream given in Example I caused a 32%
reduction of the tensile strength of cotton fabric
M83(PO4)2.5H2O _______________________ .._
H20
when subjected to the test previously described.
Using no inhibitor, that is, substituting water 40
for the aluminum phosphate, the same test gave
an 84% loss in tensile strength. The oil phase
(part I) can be varied to suit the consistency
______________ __.“, _______________ __
5.5
44.5
Tensile strength gain of 5.2%.
The corrosive e?ect of the preparations given
in the foregoing examples was determined ac
cording to the tests. described hereinbefore. It
is unlikely that any garment which might come.
desired, as can the water phase (part II), but
the ingredients of part II are the important agents 45 into contact with these preparations during use
wouldbe subjected to such drastic conditions as
in controlling‘ the anti-perspirant effectiveness
those represented by these tests. Under less
and the corrosiveness of the preparation. Ac
drastic conditions, particularly where fabrics are
cordingly, the use of 10 parts of aluminum phos
washed or otherwise cleansed after contact with
phate with a subsequent reduction of water gives
an anti-perspirant solution which shows no. col‘.-_ 50 the anti-perspirant preparation and prior to
pressing or other heat treatment, preparations
rosive effect upon cotton fabrics. In fact, the
such as illustrated by Examples 1, V, VII and IX
test (see Example II) showed a slight increase
would have av much less corrosive e?ect thereon.
in tensile strength of cotton fabric. This solu
It will be understood by chemists skilled in the
tlon and other anti-perspirant solutions and their
‘ art that a solution made by dissolving aluminum
effect on cotton fabric are noted herewith:
55 sulphate or aluminum chloride in water, and then
dissolving aluminum phosphate therein, probably
Example I!
.
Parts
Alz(SO4)a.18HaO _________________________ __. 19
AIPO; __________________________________ -_ 10
H2O
__-
_____ __
__
60 when sodium phosphate is dissolved in a solution
Parts
of aluminum sulphate, the solution contains alu
minum, sulphate, phosphate and sodium ions. A
similar condition obtains by the addition of the
‘other salts which have been referred to hereinbe
Example III
Al2(SO4)a.1BH2O _________________________ ..> 16
__.‘ _____ __. ________________________ __
4
H2O _______________________________ __,____; 55
Tensile strength loss of 2.5%.
phosphate in situ.
Therefore, in view of the diiliculty of determin
ing the nature of the various substances in the
formed therein, the solution will be designated
Parts
A12(SO4)a.18H2O _________________________ -_ 18
AlP04 _____________________________ __'_____
6
H2O ____________________________________ -_ 51
Tensile strength loss of 1.3% .
65 fore as suitable for formation of the aluminum
solution, whether added as such or presumably‘
Example IV
‘
contains aluminum, sulphate - (or chloride) and
phosphate ions, and possibly complex ions. Also,
45
_-_
Tensile strength gain of ‘6.3%.
.AlPO4
does. not contain these compounds as such, but
as a solution of the aluminum sulphate or alumi
num chloride, or other astringent aluminum-salt,
and the aluminum phosphate, whether added as
aluminum phosphate or formed therein by the
75 addition of the salt, such as sodium, calcium,
2,412,586 ,
8
magnesium. etc., phosphate, referred to herein?
and an aluminum salt from the group consisting
before.
. 01' aluminum orthophosphate and aluminum py-jv
We claim:
1. A perspirant inhibiting or retarding com
position comprising a\ water-containing vehicle,
rophosphate. the mol ratio of the aluminum phos
phate to the aluminum salt or the ?rst group be
Cl
sisting oi’ aluminum sulphate and aluminum
chloride, ‘and a corrosion inhibiting compound
prising aluminum sulphate and aluminum ortho
phosphate, the aluminum sulphate comprising
selected from the group consisting of aluminum
orthophosphate and aluminumv pyrophosphate,
ing at least one to one.
4. A perspiration inhibiting preparation com
an aluminum salt selected from the group con
at least 10% or the total preparation and the mol
10 ratio of aluminum orthophosphate to aluminum
the mol ratio of the phosphate to the salt of the
first group being at least one to one.
2. Aperspiration ‘inhibiting or retarding com
position comprising a water-containing vehicle,
an aluminum salt selected from the group con
sisting of aluminum sulphate . and aluminum
sulphate being at least one to one.
.
5. A perspiration inhibiting preparation com
prising aluminum sulphate and aluminum pyro
phosphate, the aluminum sulphate comprising at
least 10% or the total preparation and the mol
ratio or aluminum pyrophosphate to aluminum
chloride in amount equal to from 10% to 30% ' sulphate being at least one to one.
of the composition, and a corrosion inhibiting
6. A perspiration inhibiting preparation com
compound selected from the group consisting of
prising aluminum chloride and aluminum ortho
aluminum orthophosphate and aluminum pyro 20 phosphate, the aluminum chloride comprising at
phosphate, the mol ratio of the phosphate to the
least 10% of the total preparation and the mol
salt or the ?rst group being at least one to one.
ratio 01’ aluminum orthophosphate to aluminum
3. A perspiration inhibiting cosmetic cream
chloride being at least one‘to one.
containing water, 10% to 30% of a substance
selected from the group consisting of aluminum 25
sulphate and aluminum chloride, an oil phase,
EARL LEROY RICHARDSON.
KENNETH LYMAN RUSSELL.
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