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Patent 1226782 Summary

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(12) Patent: (11) CA 1226782
(21) Application Number: 465210
(54) English Title: AQUEOUS LAUNDRY PRESPOTTING COMPOSITION
(54) French Title: AGENT LIQUIDE DETACHEUR PRE-LESSIVE
Status: Expired
Bibliographic Data
(52) Canadian Patent Classification (CPC):
  • 134/3.1
(51) International Patent Classification (IPC):
  • C11D 1/66 (2006.01)
  • C11D 1/72 (2006.01)
  • C11D 3/20 (2006.01)
  • C11D 3/33 (2006.01)
(72) Inventors :
  • GIPP, MARK M. (United States of America)
(73) Owners :
  • JOHNSON (S. C.) & SON, INC. (United States of America)
(71) Applicants :
(74) Agent: BERESKIN & PARR
(74) Associate agent:
(45) Issued: 1987-09-15
(22) Filed Date: 1984-10-11
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data:
Application No. Country/Territory Date
653,865 United States of America 1984-09-25
541,201 United States of America 1983-10-12

Abstracts

English Abstract



ABSTRACT

An aqueous laundry prespotting composition which is
essentially free of solvent, having from 0.1 to 6% of
a chelating agent, from 5.0 to 40% by weight of at least
one nonionic surfactant, having an HLB in the range of
from 9.0 to 13.0 and water. The composition having a
pH of from 4.5 to 12.2.


Claims

Note: Claims are shown in the official language in which they were submitted.


- 21 -

The embodiments of the invention in which an
exclusive property or privilege is claimed are defined
as follows:

1. A laundry prespotting composition comprising:
(a) from about 0.1 to 6% by weight of a chelating
agent;
(b) from about 5 to 40% by weight of at least
one nonionic surfactant wherein the
surfactant has an HLB such that the combined
HLB for all surfactants present is within
the range of from 9 to 13; and
(c) water;
wherein the composition is substantially solvent free and
wherein the composition has a pH within the range of from
about 4.5 to 12.2.
2. The composition of Claim 1 wherein the chelating
agent is selected from the group consisting of salts of
ethylenediaminetetraacetic acid, salts of
diethylenetriaminepentaacetic acid, salts of
(N-hydroxyethyl) ethylenediaminetriacetic acid, salts of
nitrilotriacetic acid, triethanolamine, diethanolamine,
monoethanolamine, and mixtures thereof.
3. The composition of Claim 1 wherein the chelating
agent is present in an amount of from 1.0 to 4.0% by
weight.
4. The composition of Claim 1 wherein the chelating
agent is present in an amount of from 1.5 to 3.0% by
weight.
5. The composition of Claim 1 wherein the chelating
agent is selected from the group consisting of salts of
ethylenediaminetetraacetic acid, salts of
diethylenetriaminepentaacetic acid, salts of
(N-hydroxyethyl) ethylenediaminetriacetic acid, salts of
nitrilotriacetic acid and mixtures thereof.

- 22 -

6. The composition of Claim 1 wherein the chelating agent
is selected from the group consisting of
ethylenediaminetetraacetic acid disodium salt,
ethylenediaminetetraacetic acid diammonium salt,
ethylenediaminetetraacetic acid dipotassium salt,
ethylenediaminetetraacetic acid tripotassium salt,
ethylenediaminetetraacetic acid trisodium salt,
ethylenediaminetetraacetic acid tetrasodium salt,
ethylenediaminetetraacetic acid tetrapotassium salt,
ethylenediaminetetraacetic acid tetrammonium salt,
nitrilotriacetic acid trisodium salt, nitrilotriacetic acid
tripotassium salt, and mixtures thereof.
7. The composition of Claim 1 wherein the chelating agent
is selected from the group consisting of
ethylenediaminetetraacetic acid tetrasodium salt,
ethylenediaminetetraacetic acid trisodium salt,
ethylenedianinetetraacetic acid disodium salt, and mixtures
thereof.
8. The composition of Claim 1 wherein the chelating agent
is citric acid.
9. The composition of Claim 1 wherein the composition
includes an effective amount of an acid sufficient to adjust
the pH of the composition to within the range of 4.5 to 12.2.
10. The composition of Claim 1 wherein the composition has
a pH within the range of from 6.5 to 8.5.
11. The composition of Claim 1 wherein the composition has
a pH within the range of from 7.0 to 8Ø
12. The composition of Claim 1 wherein the HLB range is
from 10 to 12.
13. The composition of Claim 1 wherein the HLB range is
from 10.5 to 11.5.
14. The composition of Claim 1 wherein the nonionic
surfactant is selected from the group consisting of ethoxylated
nonylphenols, ethoxylated octylphenols, ethoxylated secondary
fatty alcohols, ethoxylated primary fatty alcohols, ethoxylated
sorbitan fatty acid esters, sorbitan fatty acid esters and
mixture thereof.




- 23 -

15. The composition of Claim 1 wherein the surfactants are
present in the amount from 5.0 to 20.0% by weight.
16. The composition of Claim 1 wherein the surfactants are
present in the amount from 7.0 to 20.0% by weight.
17. A laundry prespotting composition comprising
(a) from about 1.0 to 4.0% by weight of a chelating
agent selected from the group consisting of salts of
ethylenediaminetetraacetic acid, salts of
diethylenetriaminepentaacetic acid, salts of (N-hydroxyethyl)
ethylenediaminetriacetic acid, salts of nitrilotriacetic acid
and mixtures thereof;
(b) from about 5 to 20% by weight of at least one
nonionic surfactant selected from the group consisting of
ethoxylated nonylphenols, ethoxylated octylphenols,
ethoxylated secondary fatty alcohols, ethoxylated primary fatty
alcohols, ethoxylated sorbitan fatty acid esters, sorbitan
fatty acid esters and mixtures thereof, wherein surfactant has
an HLB such that the combined HLB for all surfactants present
is within the range of from 10 to 12; and
(c) water wherein the composition is substantially
solvent free and wherein the composition has a pH within the
range of 6.5 to 8.5.
18. A laundry prespotting composition comprising:
(a) from about 1.0 to 4.0% by weight of citric acid;
(b) from about 5 to 20% by weight of a nonionic
surfactant having an HLB such that the combined HLB for all
surfactants present is within the range from 10 to 12, said
surfactant selected from the group consisting of ethoxylated
nonylphenols, ethoxylated octylphenols, ethoxylated secondary
fatty alcohols, ethoxylated primary fatty alcohols, ethoxylated
sorbitan fatty acid esters, sorbitan fatty acid esters and
mixtures thereof; and
(c) water
the composition being substantially solvent free
and having a pH from 6.5 to 8.5.



Description

Note: Descriptions are shown in the official language in which they were submitted.


I 3~'`J~f;
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This invention relates to laundry prespotting compositions.
More particularly, this invention relates to aqueous lawn-
dry prespotting compositions having excellent stain
removal properties.


Current commercially- available prespotting compositions
fall into two categories, those based primarily upon water
and those based primarily upon solvents. The aqueous
based prespotting compositions are primarily non aerosol
formulations intended for use in trigger spray bottles or
squeeze bottles. These aqueous based prespotting combo-
sessions have good stain removal characteristics against
the so-called water-borne stains. These stains include
grape juice, mustard, grass, chocolate, clay and similar
stains.


The solvent based composition formulations typically have
been packaged in aerosol form. These solvent-based

compositions typically are more effective in removing
- oil-borne stains, such as cooking oil, fat, spaghetti
sauce, serum, grease, motor oil and the like. It is
possible to formulate solvent-based prespotting compost-
lions with reasonable water-borne stain remover.
However, it is desirable to use a composition which has
good removal for both water-borne and oil borne stains.


There have been attempt to replace the solvent with
water in prespotter compositions for both aerosol and


,

2 ,.
., .
non-aerosol formulation types. One approach is described
in U. S. Patent ~,~38,009, issued March 20, 1984. The
compositions described in this patent are emulsions
containing a salt, a non ionic surfactant, from 5 to 60%
by weight of a solvent, and water. these compositions are
described as having good stain removal properties but
these compositions require that some solvent be present
for the enhanced stain removal.

Another approach is set forth in U. S. Patent ~,079,078,
issued March 14, 197~. A typical formulation having _
certain ingredients corresponding to the teachings of that
patent is tested in Example I herein as a comparative
formulation. Such compositions require a non ionic
surfactant, an anionic surfactant, an alkanolamine, a
base, water, a fatty acid corrosion inhibitor, as oleic
acid, and optionally, an electrolyte salt to reduce gel
formation, such as sodium citrate, and a color stabilizing
agent, as citric acid in amounts of up to lo.

Most commercially available liquid prespotting formulations
are totally aqueous. These aqueous formulations exhibit
good stain removal for the water-borne stains but are
inferior to solvent based prespotters for oil removal.

Most aerosol prespotting formulations and a few liquid
formulations are totally non-aqueous. These formulations
have excellent oil-borne stain removal but are less
effective against water-borne stains. Further these
solvent products often contribute to soil redeposition.

The object to the present invention to provide an aqueous
liquid prespotting composition having superior cleaning
properties for both oil and water-borne stains.

.

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- 3 -
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Accordingly, the present invention provides a laundry
prespotting composition comprising: (a) from about Owe
to 6% by weight of a chelating agent; (b) from about
5 to about 40~ by weight of at least one non ionic surface
lent wherein the surfactant has an HUB such that the
combined HUB for all surfactants present is within the I-
range of from 9 to 13; and (c) water; wherein the
composition is substantially solvent free and wherein
the composition has a pi within the range of from about
4.5 to 12.2.

It has been surprisingly found that the aqueous prespot-
tying composition of the present invention exhibits good
cleaning including oil removal and recoil inhibition under
most conditions encountered in the home laundry. The
prespotting composition of the present invention has
cleaning properties equal to or better than solvent
containing compositions.

The compositions of the present invention are generally
liquids of varying viscosities from rather thin compost-
lions suitable primarily for use as pump spray or squeeze
bottle spray compositions to rather thick formulations
which would have to be spread on the cloth by some I`
alternate method.

Still further features and advantages of the composition
of the present invention will become more apparent
from the following more detailed description thereof.

The first component of the compositions to the present
invention is a chelating agent. It is thought that the
chelating agent functions in the composition to the
present invention to assist in removal of certain heavy
ions which inhibit the surfactancy of the non ionic
`: `

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to

; 4 .

surfactants. Also these chelating agents act in concert
with the non ionic surfactant so that the surfactant is in
the right configuration to attack oily stains from an
aqueous system. Suitable chelating gents include the
salts of ethylenediamine tetraacetic acid (ETA) such as
ethylenediaminetetraacetic acid disodium salt,
ethylenediaminetetraacetic acid diammonium salt,
e-thylenediaminetetraacetic acid trisodium salt,
ethylenediaminetetraacetic acid tetrasodium salt,
ethylenediaminetetraacetic acid tetrapotassium salt,
ethylenediaminetetraacetic acid tetrammonium salt, etc.,
the salts of diethylenetriaminepentaacetic acid (DTPA)
such as diethylenetriaminepentaacetic acid pentasodium
salt, diethylenetriaminepentaacetic acid pentapotassium
salt, etc., the salts of (N-hydroxyethyl)




-.

; 5 '

ethylenediaminetriacetic acid (HIDEOUT) such as
(N-hydroxyethyl) ethylenediaminetriac2tic acid trisodium
salt, (N-hydroxyethyl) ethylenediaminetriacetic acid
tripotassium salt, etc., the salts of nitrilotriacetic
acid (NAT) such as nitrilotriacetic acid trisodium salt,
nitrilotriacetic acid tripotassium salt, etch other
chelating agents such as triethanolamine, diethanolamine, !_
monoethanolamine, etc. and mixtures thereof. Preferred
chelating agents are the ETA and the NAT type chelating
agents especially the salts of ethylenediaminetretraacetic
acid and particularly the tetrasodium, trisodium and _
disodium salts of ethylenediaminetetraacetic acid.

typically the chelating agents are present in the
composition of the present invention in an amount of from
about 0.1 to 6% by weight. It is within this weight range
that the optimum cleaning and presetting efficiency is
obtained. It is preferred that the chelating agents be
present in the amount of from about 1.0 to I by weight
and preferable from lo to 3.0~ by weight.

The chelating agents, especially the ETA, DTPA, and HIDEOUT
types, can be added to the composition of the present
invention in the salt form, which is preferred since the -
salts are water soluble, or in the water insoluble free
acid form. If the chelating agents are added in the free
acid form, the free acids must be at least partially
neutralized to make them water soluble and form the
chelating agent salts in situ. Suitable bases to
neutralize the free acids are sodium hydroxide, potassium
hydroxide and ammonium hydroxide. Sufficient vase is
added to syllables the free acid chelating agent and to
bring the pi of the composition within the range of about
4.5 to 12.2.
Jo

2 .-
, - 6 - I

If the chelating agents are added as salts, these salts
are often quite basic, having a pi often above 10. It may
be necessary to add some acid or other pi buffering
material to the composition of the present invention to
adjust the pi to within a range of from 4.5 to 12.2 and
preferably 6.5 to 8.5 and optimum 7 to 8. Suitable acids
include citric acid, oxalic acid, acetic acid,
hydrochloric acid, phosphoric, and the like. The primary
function of the acid is to control the pi so that the
chelating agent and the surfactants can remove the stains
from the fabrics. Certain organic acids also have some
cnelatin~ properties and therefore may contribute to the
overall cleaning efficiency of the prespotting
composition. Generally the acids, if used, are present in
the compositions in the amount of from 0.2 to 2% by
weight, however the amount of acid used is not critical.
I've preferred acid is citric acid.

Citric acid may also be employed as a chelating agent,
since it possesses chelating properties. For this purpose
it is employed in cnelatiny amounts from about 1.0 to 4.0
by weight and, preferably, from 1.5 to 3.0% by weight. A
suitable base can be employed to adjust the pi of the
composition to within the preferred range from 6.5 to I
and, optimally, between 7 and 8.

Accordingly, citric acid may be employed herein as a first
component of the inventive composition to assist in
removing heavy ions and/or to act in concert with the
non ionic surfactant to aid in attacking oily stains. If
desired, it is also employed in combination with other
chelating agents of the invention, to assist in
controlling the final pi of the composition, when such
other chelating agents are added as salts.



The compositions of the present invention also include at
least one non ionic surfactant. A single non ionic
surfactant having an appropriate LO can be utilized or
mixtures of non ionic surfactants such that the HUB of the L
resulting mixture of non ionic surfactants is within the
appropriate range. It has generally been found that the
non ionic surfactant or mixture of non ionic surfactants
should hove an HUB within the range of from 9 to 13 for
optimum efficiency. It is preferred that the HUB be
between 10 and 12. The optimum LO range is from 10.5 to
11.5.

Suitable non ionic surfactants include the ethoxylated
nonylphenols such as the Surfonic N series available from
Texaco Chemicals; and the ethoxylated octylphenols
including the Briton X series available from Room & Has;
tune ethoxylated secondary fatty alcohols such as the
Tergitol~series available from Union Carbide; the
ethoxylated primary fatty alcohols suck as the Noodles
available from Shell Chemicals; the ethoxylated sorbitan
fatty acid esters such as the eons from ICY America and
the sorbitan fatty acid esters such as the Spans from ICY
America

The preferred surfactants include the ethoxylated
nonylphenols especially those having a degree of
ethyloxylation of from 3 to 10 moles of ethylene oxide,
the ethoxylated octylphenols especially those having from
3 to 10 moles of ethylene oxide and the ethoxylated fatty
secondary alcohols especially those having from 3 to 10
moles of ethylene oxide, As noted above mixtures of
non ionic surfactants, which individually have an HUB
outside the range, can be utilized so long as the
resultant HUB value of the mixture is within the range us
set forth above. It is within this LO range that the
stain removal properties of the composition of the resent
J~10tes tile marts

en
`
of
invention are at a maximum. Outside this range there is
not sufficient oil and water dispersibility to provide
suitable stain removing properties. Generally it has been
found that the non ionic surfactants which are water L
dispersible have the best stain removal properties in the
compositions of the present invention. It is thought that --
water dispersible surfactants act both against oil and
water borne stains.

Generally the composition should include from 5 to 40% by
weight of at least one non ionic surfactant and preferably
from 5 to 20% by weight and optimally 7 to 20~ by weight
of at least one non ionic surfactant.

Tune compositions of the present invention are
characterized as being substantially solvent free. By the
term "substantially solvent free is meant a composition
which contains less than 1% by weight of an organic water
immiscible solvent such as isoparaffinic hydrocarbons,
deodorized kerosene, d-limonene, the chlorinated solvents
such as perchloroethylene, ethylene chloride etc., This -
term is meant to exclude those non-polar water insoluble
solvents typically used in stain removal compositions.

The compositions of the present invention can also include
small additional amounts of other conventional materials
including perfumes, defamers, bacteriacides, bacterstats
and the like. Generally these materials are present in
amounts of less than 2% by weight based on the amount of
the composition.

Although the compositions of the resent invention are
primarily designed for use as prespotting compositions,
these compositions can also be used as laundry detergents
or cleaning agents- These compositions can be used as
heavy duty liquid laundry cleaning compositions.

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pi
The compositions of the present invention can be prepared
by any conventional means. Suitable methods include cold
blending or other mixing processes. It is not necessary
to use high shear or other strenuous mixing techniques to
prepare the compositions of the present invention.

The prespotting compositions of the present invention will r
now be illustrated by way of the following examples where
all part percentages are Dye weight and all temperatures
and degrees Celsius unless otherwise indicated.

Example A

An artificial serum soil was prepared as follows:

Part A

Weight Gyms

Palmitic Acid 5.0
Starkey Acid 2.5
Coconut Oil 7.5
Paraffin 5.0
Spermaceti 7,5
Olive Oil 10.0
Skyline 2.5
Chloresterol 2.5
Oleic Acid 5.0
Linoleic Acid 2.5
50.0

Part B
,
Oleic Acid 4.0 gyms.
Triethanolamine By gyms.

Do ".
;, - 1 0 - ,

Melt all the components of Part A together at 120-130 F.
Add Part to Part A with agitation while hot until
homogeneous. At this time, 12 grams of air filter dirt
(~200 mesh) is added and agitated for 10 minutes. From
50-100 ml of 120 F deionized water it added with
agitation and stirred for 10 minutes. From 900-950 ml (to
total 1000 ml) of 120~ F deionized water it added and
agitated until the temperature of the mixture drops to
110~ F. The mixture is agitated in a Gifford Wood
homogenizer for 10 minutes or until 120~ F. Pour the
mixture through cheesecloth and store in 100 F oven. _

Example B

Grass stain slurry is prepared by placing 50 grams of
fresh grass clippings and 500 grams of water in a blender
and gradually increasing the speed to "liquefy". Add
isopropyl alcohol as needed (up to 50 grams) to reduce
foaming and blend for I minutes. Add remainder of
isopropyl alcohol (to 50 grams total) and mix for 5
minutes. Strain through a 40 mess screen and keep
refrigerated until use.

xam?le 1

A liquid prespotting composition hazing the following
composition was prepared:
Water 84.1~,
Nonylphenol ethyloxylate
(6 moles ethylene oxide)
(Surfonic N-60) 10
Ethylenediaminetetraacetic
acid, tetrasodium salt
(40% active) 5%
Citric acid (50% active) 0.9~
100. I . -


This formulation was mixed and then placed into a squeeze
bottle having a fountain type cap for testing. The
composition had a pi of 7.9. The formulation was tested
on 4 types of white clown swatches: 100% cotton, 65~35 I-
polyester/ cotton, 50/50 polyesterfcotton, and 100%
polyester. Each swatch was stained with 7 stains, used
motor oil, mustard, rape juice, chocolate, a 20% clay
slurry, artificial serum (example A), and grass slurry
(Example B). The swatches were saturated with the above
formulation and allowed to sit for l minute. The swatches
were then washed with Tide detergent available from
Procter & Gamble with a dummy load of cotton towels. The
L
stain removal characteristics were rated on a 5 point
scale with l being essentially no removal and 5 being
complete removal. The above formulation is compared to a
liquid prespotter formulation (comparative) containing 2
sodium citrate, 8% of a Cl2-Cl5 ethoylated alcohol (7
moles ethylene oxide), 2.4% sodium zillion sulfonate and
87.6~ water. The results are shown in Table l.

TABLE l
.. _ . _ . _ _ , . . . . ..
1100% Cotton 165 Polyester/150 Polyester/ll00% Polyester
1 135 Cotton 150 Cotton
Stain Rex. l Coup. REX. l Coup. Rex. l Coup. I En. l Coup.
Used Oil 1 2.5 l 1 2 l 1 2.5 1.5 1 2
Mustard ¦ 2 2 ¦ 5 5 1 4 4 1 5 5
Grape juice 1 4 l 1 4.5 4 1 4.5 4 1 5 5
Chocolate 5 5 1 4.5 4.5 1 5 5
Clay 5 5 1 4 4 1 5 4.5
Grass 1 3 3 1 3 3 1 3 3 1 5 5
Serum 1 3.5 4 14.5 4.5 1 5 5 1 5 5
Composite 1 2.501.85 14.07 3.93 1 3.93 3.7I I 4.57 4.29
l I I
The formulation of Example l had a composite stain removal of
approximately 3.75 for all four cloth types while the comparative
composition had a composite of 3.46. The stain removal scores for
both formulations are about equal for all stains except used motor
oil. or this stain the comparative formula did not remove the stain
for any cloth type while the formulation of Example l showed improved
oil stain removal.
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; 12

Example 2

The procedure of Example 1 is repeated except that the
formulation is changed as shown in Table 2. The
formulations are tested in accordance with the procedure
of Example 1. As the stain removal scores for stains
other than used motor oil are essentially equivalent only
the results showing the increased used motor oil removal
are shown in Table 2.

TABLE 2

RUN I A I B ¦ C I _

Water 1 88.1 1 86.1 1 82.1
Surfonic N-601 1 6.0 ¦ 8.0 1 12.0
Nay ETA (40~)2 1 5.0 i 5.0 1 5.0
Citric Acid t50~) 1 0.9 1 0.9 1 0.9

Used Oil Removal
I
Cotton 1 1.5 1 2 1 3 1 _
65 Pull Cotton I 1 1 1.5 1 2
50 Pull Cotton 1 2 1 2 1 3
Polyester 1 1.5 1 2 1 2

1 Surfonic N-60 - Same as used in Example 1.
2 Nay - Tetrasodium Salt of
Ethylenediaminetetraacetic Acid.
3 Used Oil Removal - Used Motor Oil Removal as per
test described in Example 1.
As it is apparent from the above, increasing the
surfactant level increases the ability of the formulation
to remove used motor oil from a variety of fabrics.

- 13 --
;, . 'i.
Example 3

The procedure of Example 1 is followed with the exception
that the formulations as -shown in Table 3 were prepared.
For comparison, similar formulations were prepared without
tune tetrasodium salt of ethylenediamenetetraacedic acids.
As the only substantial differences between the
formulations in stain removal is in the used motor oil
removal, this was also shown in Table 3.

A LYE 3

RUN I A I B ¦ C ¦ Do I En I F4

Water 1 74.1 1 69.1 1 64.1 1 80 1 75 1 70
Surfonic ~-6~1 1 20 1 25 1 30 1 20 1 25 1 30
Nay Eddy (40%)2 1 5.0 1 5.0 1 5.0
Citric Acid (50%) 1 0.9 1 0.9 1 0.9

Used Oil Removal

Cotton 1 3 1 3.5 1 4 1 2 1 2 1 3
65 Pull Cotton 1 2 1 3 1 3.5 1 1 1 1.5 1 2
Polyester 1 3 1 4 1 3 ! 2 1 3 1 2.5
___ I .. _ I_ I , I
1 - 3 As in Table 2. --
4 Comparative

I
14 : ! i

Example 4

Procedure of Example 1 is repeated with the exception that
the formulations used in Table 4 were run.

TABLE 4 -
I r
RUN ¦ A ¦ B I C I D

Water 1 84.1 1 ~4.1 1 84.1 1 84.1
Surfonic ~-601 1 9.5 1 9.25 1 9 1 8.5 1 _
Surfonic N-31.54 1 0.5 1 0.75 1 1 1 1.5
Nay ETA (40~)2 1 5.0 ¦ 5.0 ¦ 5.0 1 5.0 1
Citric Acid (50%) 1 US I I 1 0.9 1 0.9
_ . I . -I _
used Oil Removal
I
Cotton 1 3.5 1 3.5 1 3.5 1 3.8
65 Pull Cotton 1 1.5 1 1.5 1 1.5
50 Pull Cotton I 2 1 1.5 1 1.5 1 1.5
Polyester 1 2.5 1 1.5
I _ . I I I I
1 - 3 As in Table 2
4 Surfonic ~-31.5 - Nonylphenol Ethoxylate (3.5 moles
ethylene oxide)

As apparent from 'liable 4, inclusion of small amounts of
the surfactants can increase the oil removal against
cotton but can effect its oil removal for other types of
cloth.

I
- 15 -

Example 5

In order to show the effect of different levels of
chelating agent, the formulations in Table 5 were prepared
and tested using the procedure of Example 1.
TABLE S

RUN I A I B I C ¦ D ¦ E ¦ F I G I Ho 1
T
Water 189.705l89.262l88~525l31.15 i7B.2 l72.25l72.3 l90
Nay DATA (40~)2 1 0.25 1 0.6251 1.25 ¦ 7.5 ¦10.0 112.5 115.0 1
Surfonic N-601 l10 l10 l10 110 l10 l10 l10 l10
Citric Acid ~50~)l 0.0451 0.1131 0.225¦ 1.35 1 1.8 1 2.251 2.7 1

Used Oil Removal3l
I _ I l . I _ I I I
Cotton 1 1.5 1 lo I 1.5 1 2.5 1 2.0 1 2 1 1 1 1
65 Pull Cotton 1 1 1.5 1 1.5 1 1 2 1 1 1 1 1 1
Polyester 1 1.5 1 2 1 1.5 1 2 1 1~5 1 1.5 1 1.5 1 1.5
L _ .. ! . l l Al I
1 - 3 As in liable I.
4 Comparative
As it is apparent from Table 5, at a level of from
approximately 0.5 to about 4% is optimum or best oil removal.
Although at very low levels and higher levels of ETA some oil
removal can be seen. In each of the formulations the citric acid
was adjusted to maintain the pi at approximately 7.9.

I Jo I Y J I IS '

; l o -- -

Example 6

In order to show the effect of different chelating agents
the formulations shown in Table 6 were prepared. In some
cases the pi was adjusted while in other cases the pi of
the material by itself was used.

TABLE 6

I
Run I A 1 B I _ I D i E I F I G ¦ H I I I J I K

Water 184.ll84.l188 1~5 185 185 185 185 184.l184.l184.]
Surfonic N-60l lo lo 1lQ- lo lo 110 lo lo lo lo ho - -
Nay EDNA (40~)2 ¦ 2. 5 1
Nay NAT ~40~)4 1 2. 51 5 . O I
Nay ETA l 1 1 2.01
I FAD (40%)6 ¦ 1 1 1 5.01
(N~4)2 A (40%)7 1 5.01
Nay DTPA (40%)8 l l l l I ¦ 5.01 1 ¦ 5.01
aye ala (40%)9 1 1 1 1 1 1 1 5.01 1 1 5.01
Try ietnanolamine I I I I I I i 1 5 . O I I 1 5 .
Citric Acid (50%~ 1 0.91 0.91 1 1 1 1 1 I Ply p I p
- I
Used Oil Removal
_. 1 1. 1 1 . I I I I I I I
Cotton 1 3.51 3.51 3.51 3.51 3 1 3.51 3.51 3 1 3.51 3.51 3.' _
65 Pull Cotton 1 2 1 2 1 l.51 1.51 l.51 2 1 2 1 l 1 2 1 l.51 2
Polyester 1 1.51 1.51 l.51 2 1 l.51 2 1 1.51 1.51 2
pi _ 17.8~1 8.314.751 8.91 4.5112.1112 1 9.81 7.61 7.21 8
1 - 3 As in Table 2
4 Trisodium salt of nitrilotriacetic acid
Disodium salt of ethylenediaminetetraacetic acid
6 Tetraammonium salt of ethylenediaminetetraacetic acid
7 Diammonium salt of ethylenediaminetetraacetic acid
8 Pentasodium salt ox diethylenetriaminepentaacetic acid
9 Trisodium salt of (N-hydroxyethyl) ethylenediaminetriacetic acid
lo P = to pi as listed below

;, I .

Example

In order to show the effect ox varying acids used to
adjust the phi the formulations shown in Table 7 were
prepared, using the procedure of Example 1. These
formulations were also tested as in Example 1.

TABLE 7

RUN I A ¦ B ¦ C ¦ D I E ¦ F

Water 1 84.1 1 84.1 1 84.1 1 84.1 1 84.1 1 84.1
Surfonic N_501 1 10 1 10 1 10 1 10 1 10 1 10
Nay dry (40~)2 1 5 1 5 1 5 1 5 1 5 1 5
Phosphoric Acid (85~)l I Pi
Oxalicacid I I 1 0.5
Boric Acid I I I 1 2.6
Hydrochloric Aria I I I I ¦ P
Glacial hectic I I P
pi I 12 1 it 1 6.6 1 8.0 1 7.6 -¦ 7.6
Used Oil Removal

Cotton 1 3.5 1 4 1 3.5 1 3 1 3 1 3.5
65 Pull Cotton 1 2 1 2 1 2 1 2 1 2 1 2
50 Pull Cotton 1 2 1 2 1 2 1 2 1 2 1 2
Polyester 1 2.5 1 2~5 1 2 1 2.5 1 OWE 1 2.5 Jo
. I i l I I I
1 - 3 As in Table 2.
4 p = to pi listed below.

' ? I

- 18 -

Example 8

The procedure in formulation of Example 1 was prepared
with the exception that the surfonic N60 was replaced with
the following surfactants:

RUN SURFAClA~ r

Nonylphenol ethoxylate 5 moles ethylene
oxide - Igepal C0-520

B 3 parts nonylphenol ethoxylate to moles _
ethylene oxide) (Surfonic N-40) - 2
parts nonylphenol ethoxyla~e (9.5 moles
ethylene oxide (Surfonic N 95~

C 2 parts Surfonic N-60 - 3 parts
secondary alcohol ethoxylate (5 moles
ethylene oxide) (Tergitol 15-S-5)

D Tergitol 15-S 5

E Octylphenol ethoxylate (4.5 moles
ethylene oxide) (Briton X-45)

F 2 parts C12-15 linear alcohol
ethoxylatel7 moles ethylene oxide)
(Nudely 25-73 -1 part C12-15 linear
alcohol ethoxylate(3 moles ethylene
oxide) (Nudely 25-3)

G 1 part sorbitanmonoleate ethoxylate ~20
moles ethylene oxide ITween 80) - 2
parts Surfonic N-40

H 1 port Inn 80 - 4 parts Surfonic N-40

-I olenO~ fri~Jei~arf~i

Jo
;:
-- 19 --
IT
The oil removal scores are shown in Table 8.
.
TABLE 8

RUN ¦ ¦ B I C I D ¦ E ¦ F ¦ G ¦ H
. I I I I _ 1, I I , I I
sty Wash I
Cotton 1 3.5 1 3 1 4 1 4 1 2.5 1 4 1 3.5 1 2.5 1
65 PQ1Y/35 Cotton 2 1 2 1 3 1 2 1 2 1 1.5 1 1.5 1 2
I Pulse Cotton 2 1 1 1 2 1 2 1 1 1 2 1 1.5 1 1
Polyester 1 1. 5 1 1.5 1 1.5 1 1.5 1 1.5 ! 1 1 1 1 1
end. Wash
Cotton 1 4.5 1 4.5 1 4.5 1 4.5 1 4.5 1 4.5 1 4.5 1 4.5 1
65 PQ1Y/35 Cotton 3.5 1 3.5 1 3.5 1 2.5 1 2.5 1 2.5 1 3 1 2.5 1
50 Pull Cotton 3 1 3 1 3 1 2 1 2 1 3 1 3 1 1.5 1 _
Polyester . 1 2.5 1 2.5 1 2 1 1. 5 1 1. 5 1 1.5 1 2 1 1. 5 1

; 20 ,:
, .
Example 9

The procedure of Example 1 is repeated with the following
formulation:
:, .
Water 86009~ r
Nonylphenol ethoxylate Lydia%
Citric acid (50~ active) 2.40%
Sodium hydroxide (50~ sown) 1.51%
100. ox%

The pi of the formulation is between 7 and I The
formulation is effective in removing stains as set forth
in Example 1.

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Administrative Status

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Administrative Status

Title Date
Forecasted Issue Date 1987-09-15
(22) Filed 1984-10-11
(45) Issued 1987-09-15
Expired 2004-10-11

Abandonment History

There is no abandonment history.

Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Application Fee $0.00 1984-10-11
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
JOHNSON (S. C.) & SON, INC.
Past Owners on Record
None
Past Owners that do not appear in the "Owners on Record" listing will appear in other documentation within the application.
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Document
Description 
Date
(yyyy-mm-dd) 
Number of pages   Size of Image (KB) 
Description 1993-09-25 20 620
Drawings 1993-09-25 1 16
Claims 1993-09-25 3 120
Abstract 1993-09-25 1 9
Cover Page 1993-09-25 1 16