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Patent 1235553 Summary

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(12) Patent: (11) CA 1235553
(21) Application Number: 485544
(54) English Title: STABLE LIQUID DETERGENTS CONTAINING ANIONIC SURFACTANT AND MONOSULFONATED BRIGHTENER
(54) French Title: DETERGENTS LIQUIDES STABLES A TENEUR D'AGENT TENSIO-ACTIF ANIONIQUE ET AGENT D'AVIVAGE MONOSULFONE
Status: Expired
Bibliographic Data
(52) Canadian Patent Classification (CPC):
  • 8/52
(51) International Patent Classification (IPC):
  • C11D 1/12 (2006.01)
  • D06L 4/60 (2017.01)
  • C11D 3/42 (2006.01)
(72) Inventors :
  • HALAS, LINDA A. (United States of America)
(73) Owners :
  • THE PROCTER & GAMBLE COMPANY (United States of America)
(71) Applicants :
(74) Agent: KIRBY EADES GALE BAKER
(74) Associate agent:
(45) Issued: 1988-04-26
(22) Filed Date: 1985-06-27
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data:
Application No. Country/Territory Date
627,600 United States of America 1984-07-03

Abstracts

English Abstract





STABLE LIQUID DETERGENTS CONTAINING
ANIONIC SURFACTANT AND MONOSULFONATED BRIGHTENER
Abstract of the Disclosure
Stable isotropic liquid laundry detergents contain-
ing anionic surfactant and monosulfonated brightener to
reduce brightener staining of fabrics. Monosulfonated
naphthotriazolyl stilbene brighteners are preferred.


Claims

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



- 37 -

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

1. A stable isotropic liquid laundry detergent composi-
tion comprising, by weight:
(a) from about 3% to about 50% of an anionic
synthetic surfactant; and
(b) from about 0.01% to about 1% of a monosul-
fonated brightener which represents at least about 60% of
the total brightener in the composition;
said composition containing less than about 2% of quater-
nary ammonium cationic surfactants having 2 chains, each
containing an average of from about 16 to about 22 carbon
atoms.

2. A composition according to Claim 1 wherein the
monosulfonated brightener represents from about 75% to
about 95% of the total brightener in the composition.

3. A composition according to Claim 2 wherein the
monosulfonated brightener represents from about 85% to
about 90% of the total brightener in the composition.

4. A composition according to Claim 1 comprising from
about 15% to about 25% of the anionic synthetic surfac-
tant, which comprises a C10-C18 alkyl sulfate containing
an average of from 0 to about 4 ethylene oxide units per
mole of alkyl sulfate, a C11-C13 linear alkylbenzene
sulfonate, or mixtures thereof.

5. A composition according to Claim 4 comprising from
about 0.1% to about 0.3% of the monosulfonated
brightener.

6. A composition according to Claim 5 further compris-
ing from about 4% to about 15% of a nonionic surfactant
which is a condensation product of a C12-C15 alcohol
with from about 3 to about 8 moles of ethylene oxide per
mole of alcohol.


- 38 -
7. A composition according to Claim 6 further compris-
ing from about 5% to about 20% of a C10-C22 fatty acid.

8. A composition according to Claim 7 wherein the
monosulfonated brightener is sodium 4-(2H-naphtho[1,2-
d]triazol-2-yl)-2-stilbenesulfonate.

9. A composition according to Claim 8 wherein the
monosulfonated brightener represents from about 80% to
about 95% of the total brightener in the composition.

10. A composition according to Claim 7 wherein the
monosulfonated brightener is sodium 4,4'-bis((4-anilino-
6-morpholino-1,3,5-triazin-2-yl)amino)-2,2'-stilbene-
sulfonate.

11. A composition according to Claim 1 being substan-
tially free of quaternary ammonion cationic surfactants
having 2 chains, each containing an average of from
about 16 to about 22 carbon atoms.

12. A composition according to Claim 1 being substan-
tially free of phosphate materials.

Description

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


:~355i~


STABLE LIQUID DETERGENTS CONTAINING
ANIONIC SURFACTANT AND MONOSULFONAT~D BRIGHTENER
Linda A. Hates
Technical Field
The present invention relates to stable, preferably
single-phase, isotropic liquid laundry detergents con-
twining anionic synthetic surfactant and a monosulfonated
brightener which reduces or eliminates brightener stain-
in of fabrics while maintaining an acceptable level of
whitening. Particularly preferred are monosulfonated
naphthotriazolyl stilbene (NUTS) brighteners. Preferred
compositions also contain a minor amount of a second
brightener to further improve fabric whitening. In such
compositions, the monosulfonated brightener herein should
represent at least about 60~, preferably at least about
75%, by weight of the total brightener in order to
provide the desired reduction in fabric staining.
Optical brighteners, also known as fluorescent
whitening agents, are commonly used in laundry deter-
gents. Brighteners deposit onto fabrics where they absorb ultraviolet radiant energy and remit it as a blue
light. This reduces or eliminates any yellowish cast to
fabrics and gives them a brighter appearance. However,
undesirable brightener staining can occur when liquid
detergents come in direct contact with cotton-containing
fabrics, such as during pretreatment. The present
invention reduces or eliminates such staining while
maintaining an acceptable level of fabric whitening.
Background Art
British Patent 2,028,365, Gray, published March 5,
1980, discloses built liquid detergents containing
anionic surfactants and one or more brighteners, include
in NUTS brighteners.
U.S. Patent 3,812,041, Inamorato, issued May 21,
1974, discloses unbolt liquid detergents containing
non ionic surfactants and anionic surfactants in a weight
ratio of non ionic to anionic ox at least 1. Optional
brighteners can include the NUTS type

I'

~3~3


U.S. Patent 3,959,157, Inamorato, issued May 25~
1976, discloses liquid detergents containing non ionic
surfactants, qua ternary ammonium softening agents and
optional brighteners, including NUTS brighteners.
U.S. Patent 4,430,236, Franks, issued February 7,
1984, discloses liquid detergents containing non ionic
surfactants, optional anionic surfactants, hydrogen
peroxide, brightener, and preferably ~uaternary ammonium
softening compounds. NUTS brighteners are specifically
mentioned as being useful.
Japanese Patent Application J74-017004, published
April 26, 1974, discloses liquid detergents containing
NUTS brighteners said to be stable to light.
German Patent Application 2,543,998, published April
7, 1977, discloses clear liquid detergents containing
certain diphenyl distyryl brighteners. Examples 1 and 2
are of liquid detergents containing mixtures of mainsail-
donated and disulfonated brighteners.
Summary of the Invention
The present invention relates to stable isotropic
liquid laundry detergent compositions comprising, by
weight:
(a) from about I to about 50% of an anionic
synthetic surfactant; and
(b) from about 0.01% to about 1% of a mainsail-
donated brightener which represents at least about 60% of
the total brightener in the composition;
said composition containing less than about 2% of quoter-
nary ammonium cat ionic surfactants having 2 chains, each
containing an average of from about 16 to about 22 carbon
atoms.
Detailed Description of the Invention
The compositions of the present invention comprise
from about 3% to about 50%, preferably from about 7% to
about 40%, and most preferably from about 15% to about
25%, by weight of an anionic synthetic surfactant.

~æ~3s5s3



Suitable anionic surfactants are disclosed in U.S. Patent
4,285,841, Barrel et at, issued August 25, 1981, arid in
U.S. Patent 3,929,678, Laughlin et at, issued December
30, 1975.
Useful anionic surfactants include the water soluble
salts, particularly the alkali metal, ammonium and alkyd-
olammonium (e.g., monoethanolammonium or triethanolam-
minim) salts, of organic sulfuric reaction products
having in their molecular structure an alkyd group
containing from about 10 to about 20 carbon atoms and a
sulfonic acid or sulfuric acid ester group. (Included in
the term "alkyd" is the alkyd portion of aureole groups.)
Examples of this group of synthetic surfactants are the
alkyd sulfates, especially those obtained by sulfating
the higher alcohols 5C8-C18 carbon atoms) such as those
produced by reducing the glycerides of tallow or coconut
oil; and the alkylbenzene sulfonates in which the alkyd
group contains from about 9 to about 15 carbon atoms, in
straight chain or branched chain configuration, e.g.,
those of the type described in U. S. Patents 2,220,099
and 2,477,383. Especially valuable are linear straight
chain alkylbenzene sulfonates in which the average number
of carbon atoms in the alkyd group is from about 11 to
I .
Other anionic surfactants herein are the water-
soluble salts of: paraffin sulfonates containing from
about 8 to about 24 (preferably about 12 to 18) carbon
atoms; alkyd glycerol ether sulfonates, especially those
ethers of C8 18 alcohols (e.g., those derived from tallow
and coconut oil); alkyd phenol ethylene oxide ether
sulfates containing from about 1 to about 4 units of
ethylene oxide per molecule and from about 8 to about 12
carbon atoms in the alkyd group; and alkyd ethylene oxide
ether sulfates containing about 1 to about 4 units of
ethylene oxide per molecule and from about 10 to about 20
carbon atoms in the alkyd group.


. .,

~:3~i553


Other useful anionic surfactants herein include the
water-soluble salts of esters of alpha-sulfonated fatty
acids containing from about 6 to 20 carbon atoms in the
fatty acid group and from about 1 to 10 carbon atoms in
the ester group; water-soluble salts of 2-acyloxy-
alkane-l-sulfonic acids containing from about 2 to 9
carbon atoms in the azalea group and from about 9 to about
23 carbon atoms in the Al Kane moiety; water-soluble salts
of olefin sulfonates containing from about 12 to 24
carbon atoms; and beta-alkyloxy Al Kane sulfonates con-
twining from about l to 3 carbon atoms in the alkyd group
and from about 8 to 20 carbon atoms in the Al Kane moiety
Preferred anionic surfactants are the C10-C18 alkyd
sulfates containing an average of from 0 to about 4
ethylene oxide units per mole of alkyd sulfate, C13
linear alkylbenzene sulfonates, and mixtures thereof.
The compositions herein can also contain other
synthetic surfactants known in the art, such as the
non ionic, cat ionic, ~witterionic~ and ampholytic surface
tents described in the above-cited Barrel et at and
Laughlin et at patents. Preferably, the total synthetic
surfactant represents from about 15~ to about 60%,
preferably from about 20% to about I by weight of the
composition. In addition, the anionic synthetic surface
lent preferably represents at least about 25~, more preferably at least about 30%, and most preferably at
least about 50~, by weight of the synthetic surfactant in
the composition. It is believed that such anionic
surfactant-containing systems provide a sufficiently high
level of cleaning and anti redeposition performance that
good fabric whitening can be maintained when using the
monosulfonated brighteners herein instead of more effect
live (but higher staining) brighteners.
A preferred cosurfactant, used at a level of from
about 2% to about 30%, preferably prom about 3% to about
25%, more preferably from about 4% to about 15~, by
weight of the composition, is an ethoxylated non ionic

:~2355~i3


surfactant of the formula Rl(OC2H4)nOH, wherein R is a
C10-C16 alkyd group or a C8-C12 alkyd phenol group, n is
from about 3 to about 9, and said non ionic surfactant has
an HUB (hydrophile-lipophile balance) of from about 10
to about 13. These surfactants are more fully described
in U.S. Patents 4,285,841, Barrel et at, issued August
25, 1981, and 4,284,532, Leukemia et at, issued August
18, 1981. Particularly preferred are condensation
products of C12-C15 alcohols with from about 3 to about
8 moles of ethylene oxide per mole of alcohol, eye.,
C12-C13 alcohol condensed with about 6.5 moles of
ethylene oxide per mole of alcohol. While these Nina
onto surfactants are preferably included in the present
compositions to enhance cleaning, it is believed they
also tend to syllables the NUT brighteners and prevent
them from depositing on fabrics. This can lead to
poorer whiteness maintenance in compositions in which
the non ionic surfactant comprises a major amount of the
synthetic surfactant.
Other preferred cosurfactants, used at a level of
from about 0.5% to about 3%, preferably from about 0.7%
to about I by weight, are certain qua ternary ammonium,
amine or amine oxide surfactants. The qua ternary
ammonium surfactants useful herein are of the formula:
[Wrier) o'er) ] R5N+X-
wherein R is an alkyd or alkyd bouncily group having from
about 6 to about 16 carbon atoms in the alkyd chain;
each R3 is selected from the group consisting of
-CH2CH2-, -CH2CH(CH3)-, -CH2CH(CH20H~, -CH2CH2CH2-, and
mixtures thereof; each R is selected from the group
consisting of C1-C~ alkyd, Cluck hydroxyalkyl, bouncily,
and hydrogen when y is not 0; R is the same as R or is
an alkyd chain wherein the total number of carbon atoms
of R2 plus R is from about 8 to about 16; each y is
from 0 to about 10 and the sum of the y values is from 0
to about 15; and X is any compatible anion.



I -'./

~æ3s~s3



Preferred of the above are the alkyd qua ternary
ammonium surfactants, especially the mono-long chain
alkyd surfactants described in the above formula when R5
is selected from the same groups as R4. The most pro-
furred qua ternary ammonium surfactants are the chloride bromide and methyl sulfate C8 16 alkyd trimethylammonium
salts, C8 16 alkyd di(hydroxyethyl~methylammonium salts,
the C8 16 alkyd hydroxyethyldimethylammonium salts,
C8 16 alkyloxypropyl trimethylammonium salts, and the
C,3_16 alkyloxypropyl dihydroxyethylmethylammonium salts.
Of the above, the C10-Cl4 alkyd trimethylammonium salts
are preferred, e.g., decal trimethylammonium methyl-
sulfate, laurel trimethylammonium chloride, myristyl
trimethylammonium bromide and coconut trimethylammonium
chloride and methyl sulfate.
Under cold water washing conditions, i.e., less
than about 65F 118.3C), the C8 lo alkyd trimethylam-
minim surfactants are particularly preferred since they
have lower Raft boundaries and crystallization tempera-
lures than the longer chain qua ternary ammonium surface
tents.
Amine surfactants useful herein are of the formula:
[R (OR ) y] [R (OR ) y] R N
wherein the R, R, R, R and y substituents are as
defined above for the qua ternary ammonium surfactants.
Particularly preferred are the C12_16 alkyd dimethY
amine.
Amine oxide surfactants useful herein are of the
formula:
[R (OR ) y] OR (OR ) y] R N -I 0
wherein the R , R , R , R and y substituents are also as
defined above for the qua ternary ammonium surfactants.
Particularly preferred are the C12_1~ alkyd dimethY
amine oxides.


55i~i3

-- 7 --
Amine and amine oxide surfactants are preferably
used at higher levels than the qua ternary ammonium
surfactants since they typically are only partially
protonated in the present compositions. For example,
preferred compositions herein can contain from about 0.5~
to about 1.5~ of the qua ternary ammonium surfactant, or
from about 13 to about I of the amine or amine oxide
surfactants.
The compositions herein can also contain minor
I amounts, generally less than about 2%, preferably less
than 1%, by weight of qua ternary ammonium cat ionic
surfactants having 2 chains, each containing an average
of from about 16 to about 22 carbon atoms. These surface
tents are disclosed in British Patent 2,041,g68, Murphy,
published September 19, 1979. However, the compositions
are preferably substantially free of such surfactants
because they can cause an undesirable "quit" staining of
fabrics, thereby reducing or eliminating the benefits
obtained from using the low staining monosulfonated
I brighteners herein. The dwelling chain cat ionic surface
tents also tend to complex with the anionic brighteners
and surfactants herein, reducing the effectiveness of
both materials.
Monosulfonated Brightener
The compositions of the present invention contain
from about 0.01% to about 1%, preferably from about 0.05~
to about 0.5~, more preferably from about 0.1% to about
0.3%, by weight of a monosulfonated brightener. While
not intending to be limited by theory, it is believed
I that the monosulfonated brighteners herein cause less
staining of fabrics because their lack of symmetry
reduces crystal growth and build up of brightener on
fabrics. For example, the preferred NUTS brighteners
herein have substantial substitution (i.e., naphthotri-
azalea and sulfonate groups) on one side of a stilbene
group and no substitution on the other side.



i

it



Preferred monosulfonated brighteners are of the
formulas

CH=CH - (1)
NO


I OR
I = N N = C
\ (2
N I -- SHEA = I 7 - I N
I - N/ I: =/ Jo ON - I
] .


I OH = SHEA?)

R R R

OH = OH Ho = Shari
(O
25 R R R
wherein one R per molecule is S03M; M is a compatible
cation, such as hydrogen, sodium (preferred), potassium,
ammonium, or substituted ammonium ego., moo-, do-, or
tri-ethanolammonium); and each other R is selected from
the group consisting of hydrogen, hydroxy, alkyd,
hydroxyalkyl, oxyalkyl, amino, substituted amino where
each substituent is hydroxy, alkyd, hydroxyalkyl, or ox-
alkyd, morpholino, aniline, halogen and cyan, said alkyd
groups containing from 1 to 4 carbon atoms.


Sue


Preferred brighteners are those of the above forum-
lay where the SIAM group is attached directly to the
stilbene portion of the molecule. Preferably each other
R is selected from the group consisting of hydrogen,
hydroxy, alkyd, hydroxyalkyl, amino, substituted amino
where each substituent is hydroxy, alkyd or hydroxyalkyl,
morpholino and amilino, said alkyd groups containing from
1 to 3 carbon atoms. In a particularly preferred bright
ever of formula (1), each other R is hydrogen, i.e.,
sodium 4-(2H-naphtho [1,2-d~ triazol-2-yl~-2-stilbene-
sulfonate, which is commercially available as Tin opal RUBS
from Ciba-Geigy. Preferred brighteners of formula (2)
are those wherein the other R attached to the stilbene
portion of the molecule is hydrogen, one R attached to
the treason rings is aniline and the other R is depth-
nolamino, morpholino, methylhydxoxyethylamino, 2-hydroxy-
propel amino, or aniline. Preferred brighteners of
formula (3) and (4) are those wherein the other R's are
all hydrogen.
Preferred compositions herein also contain a minor
amount of a second brightener to improve fabric whiten-
in In such compositions, the monosulfonated brightener
herein represents from about 60~ to about 99%, preferably
from about 75% to about 95%, more preferably from about
80% to about 95~, most preferably from about 85~ to about
90%, by weight of the total brightener in order to
improve whitening while reducing staining to an accept-
able degree. Suitable co-brighteners include any of
those known for use in detergent compositions. Examples
are disclosed in U.S. Patent 3,812,041, Inamorato, issued
May 21, 1974.
Other Components
The compositions of the present invention preferably
contain from about 25% to about 65%, more preferably from
about 30% to about 60~, most preferably from about 40% to
about 55%, by weight of water.



Jo

~23~i~i53


-- 10 --
The compositions also preferably contain from about
3% to about 30~, more preferably from about 5% to about
20%, by weight of a fatty acid containing from about 10
to about 22 carbon atoms. The fatty acid can also
contain from about 1 to about 10 ethylene oxide units in
the hydrocarbon chain. Preferred are saturated fatty
acids containing from about 10 to about 14 carbon atoms.
In addition, the weight ratio of ClO-Cl2 fatty acid to
C14 fatty acid should be at least 1, preferably at least
1 . 5 .
Suitable saturated fatty acids can be obtained from
natural sources such as plant or animal esters (e.g.,
stripped palm kernel oil, stripped palm oil and coconut
oil) or synthetically prepared ego.; via the oxidation
of petroleum or by hydrogenation of carbon monoxide via
the Fisher~Tropsch process). Examples of suitable
saturated fatty acids for use in the compositions of this
invention include caprice Laurie, myristic, coconut and
palm kernel fatty acid. Preferred are saturated coconut
fatty acids, from about 5:1 to 1:1 (preferably about 3:1)
weight ratio mixtures of Laurie and myristic acid,
mixtures of the above with minor amounts leg., 10~-30~
of total fatty acid) of oleic acid; and stripped palm
kernel fatty acid.
The compositions herein also preferably contain up
to about 25~, preferably from about I to about 10~, by
weight of a detergent builder material. Detergent
builders are described in U.S. Patent 4,321,165, Smith et
at, issued March 23l 1982. However, the compositions
preferably contain less than about lo, more prefer-
ably less than about 5%, of phosphate materials. Most
preferably, the compositions are substantially free of
phosphates. Preferred builders are the polycarboxylate
materials described in U.S. Patent 4,284,532r Leukemia et
at, issued August 18, 1981. Citric acid is particularly
preferred.

~23~53



Other optional components for use in the liquid
detergents herein include enzymes, enzyme stabilizing
agents, palisades, soil removal agents, anti redeposition
agents, suds regulants, hydrotropes, pacifiers, anti-
oxidants, bactericide, dyes perfumes, and other bright-
enters known in the art. Such optional components
generally represent less than about 15%, preferably from
about 2% to about 10%, by weight of the composition.
The following examples illustrate the compositions
of the present invention.
All parts, percentages and ratios used herein are by
weight unless otherwise specified.
EXAMPLE I
The fabric staining tendency of various brighteners
was evaluated in the following composition.
Component Wt. %
C13 linear alkylbenzene sulfonic acid 7.2
C14 15 alkyd polyethoxylate (2.25~
sulfuric acid 10.8
C12 13 alcohol polyethoxylate (6.5)* 6.5
C12 alkyd trimethylammonium chloride 1.2
C12-14 fatty acid 13.0
Oleic acid 20 0
Citric acid an hydrous 4.0
25 Di~thylenetriamine pentaacetic acid 0.23
T 15 18** 1.5
Monoethanolamine 2.0
Sodium ion 1.66
Potassium ion 2.65
30 Propylene glycol 7.25
Ethanol 7.75
Formic acid 0.66
Brightener As indicated
Minors and water Balance to 100
*Alcohol and monoethoxylated alcohol removed.
**Tetraethylene pentaimine ethoxylated with 15-18 moles
(avg.) of ethylene oxide it each hydrogen site.


Lowe

- 12
Brightener
A = 0.13% disodium 4,4'-bis((4-anilino-6-methylhydroxy-
ethylamino-1,3,5-triazin-2-yl)amino)-2,2'-stilbenee
disulfonate
-~0.076~ dipotassium 4,4'-bis(4-phenyl-1,2,3-
txiazol-2-yl~stilbene-2,2'-disulfonate
B = 0.2% KIWI. Fluorescent Brightener 230
C = 0.2% of a hexasulfonated stilbene brightener
D = 0.2% tetrasodium 4,4'-bis((4-[bis(2-hydroxyethyl)-
amino]-6-(p-sulfoanilino) -1,3/5-triazin~2~yl)-
amino)-2,2'-stilbene disulfonate
E = 0.2% sodium 4-(2H-naphtho [1,2-d] triazol yule)-
2-stilbenesulfonate)
The above brighteners are preferably added to the
composition as a premix containing, on a finished product
basis, 2% monoethanolamine, 2% alcohol polyethoxylate and
2% water, to aid their solubilization.
samples containing the above brighteners were
applied to 100% cotton swatches (unbrightened unless
otherwise noted), both damp and dry, fox lo minutes, and
to dry swatches for 1 hour. The swatches were then
washed, dried and graded under ultraviolet light for
brightener staining by a panel of expert graders, using
the following scale.
O = no visible stain
T = trace of stain
1.0 = very light stain
1.5 = light stain
2.0 = medium light stain
2.5 = medium stain
3.0 = heavy stain
The results, after averaging the grades, were as
follows.



:~3~5~3


- 13 -
Fabric Brig~tenerGrade
Dry Damp Dry
lo mix 10 mix l ho
Prebrightened
5 shirt A 2.5 2.3 2.3
s 3.1 3.3 3.3
- C 2.2 2.7 1.9
D 3.2 3.5 3.1
" E 0 T T
underwear A 2.1 2.8 2.3
" B 2.7 3.0 3.1
C 1.3 2.3 1.3
" D 2.8 3.5 2.3
1- E T 1.0 T
Coarse weave
cotton A 3.6 3.0 3.3
" B 4.0 3.7 3.7
" C 2.6 2.3 2.3
1- D 3.2 3.3 3.4
" E 1.3 1.3 1.3
Cotton sweater A 2.4 2.8 2.5
" B 3.3 3.3 3.2
" C 2.2 2.4 2.2
" D 3.2 3.1 3.2
25 11 E 1.0 1.0 1.0
Blue cotton A 3.5 2.6 2.8
" B 2.7 3.1 3.3
" C 1.0 1.6 1.0
" D 2.1 2.7 2~7
" E 0 0 0
Brightener E of the present invention caused much
less staining of cotton fabrics than the other
brighteners.
EXAMPLE II
Example I was repeated (10 minute application only)
using the following brighteners.

So 3


- 14 -
A = 0.13g disodium 4,4'-bis((4-anilino-~-methylhydroxy-
ethylamino-1,3,5-triazin-2-yl~amino)-2,2'-~tilbenee
disulfonate
+0.076% dipotassium 4,4'-bis(4-phenyl-1,2,3-
triazol-2-yl)stilbene-2,2'-disulfonate
B = 0.2% KIWI. Fluorescent Brightener 71 (a disulfonate)
C = 0.2% KIWI. Fluorescent Brightener 230
D = 0.2% of an anionic stilbene brightener
E = 0.2% sodium 4-(2H-naphtho [1,2-d~ triazol-2-yl)-2-
stilbenesulfonate)
Fabric Brightener Grade
Dry/10 min. Damp/10 min.
Prebrightened
shirt A 1.9 2.7
15" B 1.8 2.8
I C 2.5 3.5
" D 2.0 3.3
" E 0 T
Underwear A 1. 8 1. B
20" B 1.7 2.2
" C 2.3 2.8
" D 2.0 2.5
" E 0 0
Coarse weave
kitten A 2.8 2.8
" B 2.3 2.9
" C 3.2 3.2
" D 2.8 2.7
" E T T
30 Cotton sweater A 2.5 2.6
" B 2.7 2.4
" C 3.1 3.1
" D 3.1 3.1
" E T T





- 15 -
Blue cotton A 1.9 1.8
B 1.8 1.8
" C 2.5 2.
" D 2.0 202
" E 0 0
White T-shirt A T 1.0
" B 0.5 1.0
" C 1.3 1.3
" D 0.5 1.2
" E o o
In the above testing, Brightener E of the present
invention caused much less staining of cotton fabrics.
EXAMPLE
Various brighteners were again evaluated as
described in Example I, except using the following
grading scale.
O = no visible stain
T = possible trace
1 = very slight stain
2 = light but definite stain
3 = very visible stain
4 = stained the most possible
Brightener
A = OWE% disodium 4,4'-bis((4-anilino-6-methylhydroxy-
ethylamino-1,3,5-triazin-2-yl)amino)-2,2'-stilbenee
disulfonate
+0.076% dipotassium 4,4'-bis(4-phenyl-1,2,3-triazol-
2-yl)stilbene-2;2'-disulfonate
B = 0.15% sodium 4-(2H-naphtho [1,2-d] triazol-2-yl)-
2-stilbenesulfonate) 0.05% of dipotassium 4,4'-
bis(4-phenyl-1,2,3-triazol-2-yl)stilbene-2,2l-disuu-
lfonate
C = 0.18~ sodium 4-(2H-naphtho [1,2-d] triazol-2-yl)-
2-stilbenesulfonate) 0.02% of dipotassium 4,4'-
bis(4-phenyl-1,2,3-triazol-2-yl)stilbene-2,2'-di-
sulfonate

I


- 16 -
D = 0.2% sodium 4-(2~-naphtho [1~2-d] triazol-2-yl)-
2-stilbenesulfonate)
Fabric Brightener Grade
10 mender
Prebrightened
shirt A 4.0
I B
" C 1.5
" D T
10 Underwear A 3.0
" B 2.0
" C 1.0
" D T
Coarse weave
kitten A 4.0
" B 3.0
" C 2~0
" D 1.0
Cotton sweater A 4~0
20 " B 2.0
" C 1.0
" D T
Blue cotton A 3.0
" B T
25 " C 0
" D 0
White T-shirt A 2.3
B 0
" C O
30 " D 0

Brighteners B (with 75% of total brightener being
D), C (with 90% of total brightener being D), and D of
the present invention again caused less staining of
cotton fabrics.


~23ss~



EXAMPLE IV
The following brighteners were evaluated, as
described in Example III.
A = 0.13% disodium 4,4'-bis((4-anilino-6-methylhydroxy-
ethylamino-1,3,5-triazin-2-yl~amino~-2,2'-stilbenee
disulfonate
+0.076% dipotassium 4,4'-bis(4-phenyl-1,2,3-tria-
zol-2-yl)stilbene-2,2'-disulfonate
B = 0.1~ sodium 4-(2H-naphtho [1,2-d] triazol-2-yl)-2-
stilbenesulfonate~
C = 0.15% sodium 4-(2H-naphtho [1,2-d] triazol-2-yl)-2-
stilbenesulfonate)
D = 0.2~ sodium 4-(2H-naphtho ~1,2-d] triazol-2-yl)-2-
stilbenesulfonate)
15 Fabric Brightener Grade
10 mender
Prebrightened
shirt A 3.5
B 0
" C 0
" D 0
Underwear A 3.5
'I B 0
" C O
" D 0
Coarse weave
cotton A 3.5
" B lo
" C 1.5
" D 1.5
Cotton sweater A duo
" B lo
" C 1.0
' D lo


~Læ~5s~3


- 18 -
Blue cotton A 3.0
B 0
" C O
" D 0
White T-shirt A lo
" B 0
" C O
.. D
The above results show that Brighteners By C and D
of the present invention caused little or no staining at
levels between Oily and 0.2%.
EXAMPLE V
The following brighteners were evaluated as
described in Example III under various pretreatment times
and conditions.
A = 0.13% disodium 4,4'-bis~(4-anilino-6-methylhydroxy-
ethylamino-l,3,5-triazin-2-yl)amino3-2,2'-stilbQnee
disulfonate
+0.076% dipotassium 4,4'-bls~4-phenyl-l,2,3-tria-
zol-2-yl3stilbene-2,2'-disulfonate
B = 0.2% sodium 4-(2H-naphtho 11,2-d] triazol-2 yule-
stilbenesulfonate)
C = 0.18% sodium 4-(2H-naphtho lid triazol-2-yl~-2-
stilbenesulfonate) + 0.02~ disodium Boyce-
25 anilino-6-methylhydroxyethylamino-l,3,5-triazin-2--
yl)amino)-2,2'-stilbene disulfonate
D = 0.15% sodium 4-(2H-naphtho [1,2-d] triazol-2-yl) 2-
stilbenesulfonate) + 0.05~ disodium Bessel-
anilino-6-methylhydroxyethylamino-l,3,5-triazin-2--
yl)amino)-2,2'-stilbene disulfonate
After lo minutes on Dry Fabric
Fabric Brightener Pretreat Condition**
l 2 3 4
Cotton sweater A 4.0 4.0 3.5 3.5
" B lo lo T T
" C 2.0 2.0 2.0 2.0
" D 3.0 3.0 2.0 2.0

5~3


-- 19 --
Coarse weave
cotton A 4.0 4.0 3.5 4.0
" B 1.0 1.0 1.0 1.0
" C 200 2~5 2.0 1.5
" D 3.0 3.0 3.0 2.5
White cotton pants A 4.0 4.0 4.0
" B 1.0 1.0 T
" C 2.0 1.5 2.0
" D 3.0 2.0 2.5
10 After 10 minutes on Damp Fabric
Fabric Brightener Pretreat Condition**
1 2 3 4
Cotton sweater A 4.0 4.0 4.0 3.5
" B 1.0 T T 1.0
" C lo 1.0 1.0 2.0
" D 3.0 2.0 2.0 2.0
Coarse weave
cotton A 4.0 4.0 4.0 4.0
" B 1.0 T 1.0 1.0
" C 2.5 2.0 2.0 2.0
" D 3.0 3.0 3.0 3.0
White cotton pants A 4.0 4.0 4.0
" B 1.0 T T
" C 2.0 1.5 1.0
" D 3.0 2.5 2.0
Overnight on Dry Fabric
Fabric Brightener Pretreat Condition**
1 2 3 4
Cotton sweater A 4.0 3.0 4.0 4.0
" B 1.0 1.0 1.0 1.0
" C 2.5 2.0 2.5 2.0
" D 3.0 3.0 3.0 3.0
Coarse weave
cotton A 4.0 4.0 4,0 4.0
" B 1.5 2.0 1.0 2.5
" C 2.0 3.0 2.0 3.0
" D 3.0 3.0 3.0 3.0

55~;3


- 20 -
White cotton pants A 4.0 4.0 4.0 3.5
B 1.0 1.0 2.0 1.0
" C 2.5 2.0 2.0 1.5
" D 3.0 2.0 3.0 1.5
Gray corduroy pants Aye 3.5 2.5
" B 0.5 1.5 1.0
" C 1.5 1.5 1.5
" D 2.0 1.5 1.5
Unbleached muslin
tablecloth A 4.0 4.0 4.0
" B 2.0 2.0 2.0
" C 2.5 2.5 3.0
" D 3.0 3.0 3.0
Overnight on Damp Fabric
15 Fabric Brightener Pretreat Condition**
1 2 3 4
Cotton sweater A 4.0 4.0 4.0 4.0
" B 1.5 2~5 2.0 T
" C 2.5 2.5 3.0 2.0
20 " D 3.5 3.0 3.0 3.0
Coarse weave
cotton A 4.0 4.0 4.0
" B 1.5 2.0 2.0 2.5
" C 2.5 3.0 3.0 3.0
25 " D 3.0 3.0 3.0 OWE
White cotton pants A 4.0 4.0 4.0 3.5
" B 2.0 1.0 1.5 T
" C 2.0 2.0 2.0 1.5
" D 2.5 3.0 3.0 2.5
grow corduroy pants A 4.0 3.5 3.5
" B 2.5 2.0 2.0
" C 2.5 2.0 2.0
" D 3.0 3.0 2.0



553



Unbleached muslin
tablecloth A OWE 4.0 4.0
" B 3.0 2.0 2.5
" C 3.0 3.0 3.0
" D 3.0 3.0 3.5
**l= 1 ml of product applied
2= 1 ml of product applied + rub 5 times
3= 2 ml of product applied scrub for 10 seconds
4= 1 ml of product applied + rub rinse
Brighteners B, C (with 90% of total brightener
being By, and D (with 75% of total brightener being B) of
the present invention provided less staining of cotton
fabrics.
EXAMPLE VI
Brightener staining was evaluated as described in
Example III using the following compositions.
Composition A = a commercially available detergent
believed to contain the following components.
Component Wt. %
C11 3 linear alkylbenæene sulfonate 17.5
C12 15 alcohol polyethoxylat~8) 7.0
Sodium citrate 10.1
Zillion sulfonate 5.2
Monoethanolamine 2.0
25 Methyl cellulose 0.7
Disodium 4,4'-bis((4-anilino-
6-morpholino-1,3,5-triazin-2-yl)
amino)-2,2'-stilbene disulfonate 0.05
Sodium 4-(2H-naphtho [1,2-d] triazol-
2-yl)-2-stilbenesulfonate 0.04
Water -I minors Balance to 100
Composition B
Component Wt._%
C12_13 alcohol polyethoxylate ~6.5) 21.5
Sodium C12 14 alcohol polyethoxylate
I sulfate 11.6

5~3



- 22 -
Ethanol 10.0
Disodium 4,4'-bis((4-anilino-
6-methylhydroxyethylamino-1,3,5-
triazin-2-yl)amino) 2,2'-stilbene
disulfonate 0.21
Waxer + minors Balance to lo
Composition C = Composition B except replace India
acted brightener with 0.2% of sodium 4-i2H-naphtho[1,2-d]
triazol-2-yl)-2-stilbenesulfonate.
Composition D = Composition B except replace India
acted brightener with 0.13% disodium 4,4'-bis((4-anilino-
6-methylhydroxyethylamino-1,3,5-triazin-2-yl)aminoowe'-
stilbene disulfonate and 0.076~ of dipotassium Boyce-
(4-phenyl-1,2,3-triazol-2-yl)stilbene-2,2'-disulfoovate.
Composition E = Composition of Example I with 0.13~
of disodium 4,4'-bis((4-anilino-6-methylhydroxyethyl-
amino-1,3,5-triazin-2-yl)amino)-2,2'-stilbene disulfonate
and 0.076~ of dipotassium 4,4'-bis(4-phenyl-1,2,3-tria-
zoo 2-yl)stilbene-2,2'-disulfonate.
Composition F = Composition of Example I with 0.15%
of sodium 4~(2H-naphtho[1,2-d] triazol-2-yl)-2-stilbene-
sulfonate and 0.05% of disodium 4,4'-bis((4-anilino-6-
methylhydroxyethylamino-1,3,5-triazin-2-yl)amino)--2,2'-
stilbene disulfonate.
Composition G = Composition of Example I with 0.15%
of sodium 4-(2H-naphtho[1,2-d] triazol-2-yl)-2-stilbene-
sulfonate and 0.02% of disodium 4,4'-bisl(4-anilino-6-
methylhydroxyethylamino-1,3,5 treason yl)amino)-2,2'-
stilbene disulfonate.
Composition H = Composition of Example I with 0.15~
of sodium 4-(2H-naphtho[1,2-d] triazol-2-yl)-2-stilbene-
sulfonate
The results were as follows.



~3~i553



- 23 -
Fabric Composition Grade
10 mender overnight/damp
Cotton sweater A 3.0 3.3
" B 3.0 4.0
" C T 2.8
D 3.5 4.0
" E 4.0 4.0
" F 3.3 3.0
" 2.3 2.5
" H 1.0 2.5
Coarse weave
cotton A 3.0 3.5
" B 3.0 4.0
" C T 2.3
" D 3.5 3.5
" E 4.0 4.0
" F 3.0 3.0
G 2.5 3.0
" H 1.3 2.3
20 White T-shirt A 1.5 1.0
" B 1.5 4.0
" C 0 2.0
" D T 3.0
" E 1.0 3.0
25 if F 1.0 2.5
" G T 2.0
" H 0 2.0
Compositions C, G and H of the present invention
caused less staining of cotton fabrics than the other
compositions. Composition F of the invention caused less
staining than Composition E, and about the same level of
staining as Composition A even though F contained more
than twice the level of brightener in A.




.

- 24 -
EXAMPLE VII
Brightener staining was evaluated as described in
Example VI on a wide variety of fabrics, using the
following compositions.
Composition A = Composition E from Example VI
Composition B = Composition H from Example VI
Composition C = Composition B from Example VI
Composition D = Composition B from Example VI,
except replace indicated brightener with the brightener
mixture of Composition G of Example VI.
Composition E = Composition G from Example VI.
The results were as follows.
Fabric Composition Grade
10 min/dr~overnight/damp
Polycotton
(84% C) A 2.0 3.0
" B O T
" C 3.0 4.0
D 2.0 3.0
20 " E T 2.5
Coarse weave
cotton A 4.0 4.0
'I B 1.0 2.0
" 3.0 3.0
25 " D 200 3.0
" 3.0 3.0
Cotton denim A 3.0 4.0
'I B 0 0
" C 3.5 3.5
30 " D 2.0 2.0
if E 1.0 1.5
Polycotton
(50~ C) A 0 2.0
" B O T
35 " C 0 2.0
" D 0 0
" E 0 T

~3~5~3~


- 25 -
Underwear A 3.5 4.0
" B T 2.5
" C 4.0 4.0
" D 3.0 3.5
5 " E 2.0 3.0
Muslin A 4.0 4.0
B 1.0 2.5
" C 4.0 I
" D 2.0 3.0
10" E I 3.0
Muslin A 3.5 3.5
" B 0 1.0
" C 4.0 4.0
" D 200 2.0
15" E 2.0 2.0
Silk A 2.0 4.0
B 1.0 3.0
C 1.0 1.5
" D T 1.5
201 E 1.0 3.0
Rayon A 4.0 4.0
B 1.0 2.0
C 4.0 4.0
if D 3.0 3.0
251 E 3.0 3.5
On polycotton (35% C), wool, polyester and triage-
late fabrics, all grades were "0" except for grades oft for overnight contact of Composition A on polycotton
(35~ C), D on wool, and B and E on triacetate, and for 10
minute contact of Composition E on triacetate.
The above results show that Compositions B, D and E
of the present invention cause less staining on a variety
of fabrics.
EXAMPLE_VII
Brightener staining was evaluated as described in
Example III, using the following brighteners.


it


- 26 -
A = 0.13% disodium 4,4'-bis(~4-anilino-6-methylhydroxy-
ethylamino-1,3,5-triazin-2 yl)amino)-2,2'-stilbene
disulfonate
+0.076% dipotassium 4,4'-bis(4-phenyl-1,2,3-triazol-
2-yl)stilbene-2,2' disulfonate
B = 0.15% sodium 4-(2H-naphtho [1,2-d] triazol-2-yl)-
2-stilbenesulfonate)
C = B + 0.01% disodium 4,4'-bis((4-anilino-6-methylhy-
droxyethylamino-1,3,5-triazin-2-yl)amino)-2,2'-
stilbene disulfonate
D = B 0.015% disodium 4~4'-bis((4-anilino-6-methyl-
hydroxyethylamino-1,3,5-triazin-2-yl)amino)-2,2'-
stilbene disulfonate
E = B + 0.02% disodium 4,4'-bis((4-anilino-6-methyl-
hydroxyethylamino-1,3,5-triazin-2-yl)amino~-2,2'-
siilbene disulfonate
FabricComposit_on Grade
10 min/dryovernight/damp
Coarse weave
cotton A 3.5 4.0
" B 1.0 1.5
" C 2.0 2.5
" D 2.0 2.0
" E 2.0 2.0
25 Cotton sweater A 3.8 4.0
" B T 2.0
" C 1.5 3.0
" D 1.8 2.0
" E 1.5 2.0
30 Unbleached muslin A 3.0 OWE
" B 0.5 2.3
" C 1.0 1.5
" D 1.5 2.0
" E 1.5 2.3


~;~35~53
. .


Underwear A 3.0 4.0
s T 3.0
" C 1.3 3.0
" D 1.3 3.0
" E 1.3 3.0
White T-shirt A 1.8 3.0
" B 0 T
" 0 1.3
" D 0 1.0
" E T 1.8
Brighteners B, C, D and E of the invention caused
less staining than Brightener A.
EXAMPLE IX
Brightener staining was evaluated as described in
Example VI using the following compositions.
Composition = Composition E of Example VI.
Composition B = Composition G of Example VI.
Composition C
Component Wt. %
20 C13 linear alkylben~ene sulfonic acid 7.2
C14_15 alkyd polyethoxylate (2.25)
sulfuric acid 10.8
C12 13 alcohol polyethoxylate (6.5)* 5.0
C12 alkyd trimethylammonium chloride 1.2
25 C12 14 fatty acid 10.0
Citric acid (an hydrous) 4.0
Diethylenetriarnine pentaacetic acid 0.23
15-18** 2.0
Monoethanolamine 2.0

30 sodium ion 1.66
Potassium ion 2.65
Propylene glycol 2.5
Ethanol By
Formic acid 0.66



~3~55i3

- 28 -
Disodium 4,4'-bis((4-anilino-6-
methylhydroxyethylamino-1,3~5-
triazin-2-yl)amino)-2,2l-
stilbene disulfonate 0.13
Dipotassium 4,4'-bist4-phenyl-
1,2,3-triazol-2-yl)stilbene-
2,2'-dlsulfonate 0~076
Minors and water Balance to 100
*Alcohol and monoethoxylated alcohol removed.
**Tetraethylene pentaimine ethoxylated with 15~18 moles
(avg.) of ethylene oxide at each hydrogen site.
Composition D = Composition C, except replace
indicated brighteners with 0.15% of sodium 4-(2H-
naphtho[l,2-d] triazol-2-yl)-2-stilbenesulfonate and
0.02% of disodium 4,4'-bis((4-anilino-6-methylhydroxy-
ethylamino-1,3,5-triazin-2-yl)amino)-2,2'-stilbenee
disulfonate.
Composition E = Composition C, except replace
indicated brighteners with 0.15% of sodium 4-(2H-naphtho-
[1,2-d] triazol-2-yl)-2-stilbenesulfonate.
The results were as follows.
FabricCvmposition Grade
10 mender overni~ht/damp
Coarse weave
cotton A 3.5 4.0
" B 2.0 2.5
" C 4.0 4.0
" D 2.0 2.0
" E 1.0 1.5
30 Cotton sweater A 3.5 3.5
" B 1.5 2.5
" C 2.5 3.5
" D 1.5 1.8
" E T 1.5


So
, ,.

- 29 -
Unbleached muslin A OWE 3.5
" B 1.8 2.0
" C 3.0 3.5
" D 1.0 2.0
S " E T 2.0
Underwear A 2.5 4.0
" B 1.5 2.5
" C 2.5 3.8
" D 1.5 2.5
" E 0 2.5
White T-shirt A T 2.5
" B 0 1.0
" C T 2.5
" D 0 lo
" E 0 T
Compositions B, D and E of the invention all caused
less staining of the cotton fabrics.
EXAMPLE X
Brightener staining was evaluated as described in
Example IX using the following compositions.
Composition = Composition C of Example IX
Composition = Composition E of Example IX
Composition C = Composition D of Example IX
Composition D = Composition C of Example IX,
except replace indicated brighteners with 0.2~ of sodium
4,4'-bis((4-anilino-6-morpholino-1,3,5-triazin-2-yyule-
amino) 2,2'-stilbene sulfonate.
Composition E = Composition C of Example IX, except
replace indicated brighteners with 0.2% of 4,4' Bessel-
30 anilino-6-morpholino-1,3,5-triazin-2-yl)amino)-2l22'-
stilbene. (Brightener not solubilized in composition.)
Composition F = Composition C of Example IX, except
replace indicated brighteners with 0.2% of disodium
4,4'-bis((4-anilino-6-morpholino-1,3,5-triazin-2-yye)-
amino)-2,2'-stilbene disulfonate.

Sue

. .

- 30 -
Composition G = Composition D, except with only
0.15% of the indicated brightener.
Composition H = Composition F, except with only
0.15% of the indicated brightener.
The results were as follows.
Fabric Composition Grade
10 mender overnight/damp
Coarse weave
cotton A 4.0 4.0
" B 1.5 2.0
" C 2.5 2.5
D 2.0 3.0
" E 4.0 1.5
" F 4.0 4.0
I. G 1.5 3.0
H 2.0 4.0
Cotton sweater A 4.0 4.0
" B 1.0 2.5
" C 1.5 3.0
" D 2.5 3.5
" E 2.0 1.5
" F 4.0 4.0
" G 2.5 3.0
.0 4.0
25 Unbleached muslin A 3.5 4.0
" B 0 2.5
.. C 1.5 3.5
" D 2.0 3.5
if E 0 1.0
" F 3.5 4.0
" G 2.5 2.5
" H 3.0 3.5
Underwear A 2.0 4.0
" B T 2.0
" C T 2.5
if D T 3.0

355~i3

-- 31 --
" E T 0
" F 2.5 4.0
" G 2.0 3.0
" H 3.0 4.0
White T-shirt A 0 3.0
" B 0 0
" C 0 1.5
" D 0 2.5
" E 0 0
" F T 3.0
" 0 3.0
" H 0 3. 0
Compositions By C, D and G of the present invention
caused less staining of the cotton fabrics. While the
preferred monosulfonated brightener in Composition B
causes less staining than the brightener in I, the
brightener in G provides better whitening performance.
EXAMPLE XI
Brightener staining was evaluated as described in
Example IX using the following compositions.
Composition A = Composition C of Example IX
Composition B = Composition E of Example IX
Composition C = Composition D of Example IX
Composition D = Composition C of Example IX,
except replace indicated brighteners with 0.2~ of
disodium 2,2-(4,4 7 -biphenylene divinylene)-dibenzene
sulfonate.
Composition E = Composition C of Example IX, except
replace indicated brighteners with 0.12~ of sodium
4-(2H-naphtho[1,2-d] triazol-2-yl)-2-stilben~sulfonate
and 0.06~ of disodium 2,2~(4,4'-biphenylene divinylene)-
dibenzenesulfonate.
Composition _ = Composition C of Example IX, except
replace indicated brighteners with 0.15% of sodium
4-(2H-naphtho[1,2-d] triazol-2-yl)-2-stilbenesulfonate
and 0.02% of disodium 2,2-(4,4'-biphenylene divinylene)-
dibenzenesulfonate.

~3~53
.. ..

- 32 -
Composition G = Composition C of Example IX, except
replace indicated brighteners with 0.096% of sodium
4-(2H-naphtho[1,2-d] triazol-2-yl)-2-stilbenesulfonate
and 0.088~ of disodium 2,2-(4,4'-biphenylene divinely-
S ene)-dibenzenesulfonate.
The results were as follows.
Fabric Composition Grade
10 min/dryoverni~ht/damp
Coarse weave
cotton A 3.5 4.0
" B 1.5 2.0
" C 2.0 2.5
" D 3.0 4.0
" E 2.5 2.0
I' F 2.0 1.5
" G 4.0 2.5
Cotton sweater A 3.0 4.0
" B 1.0 2.0
" C 1.0 2.5
" D 3.0 4.0
" E 2.5 3.5
" 2.5 2.0
" G 2.5 2.5
Unbleached muslin A 2.0 3.0
" B T T
" C T 1.5
" D 2.5 3.5
" E 1.0 2.0
" F T 1.5
" G 1.5 1.0
Underwear A 1.5 3.5
" B 0 1.0
" C T 1.0
" D 2.0 3.5
" E T 2.0
" F T 2.0
" G 1.5 2.5

~35~53
. .

- 33 -
White T-shirt A T 2.5
B 0 T
" C 0 1.0
" D T 3.0
" E 0 1.0
" F T T
" G T 2.0
Compositions B, C, E and F of the present invention
caused less staining of the cotton fabrics.
EXAMPLE XII
Brightener staining was evaluated as described in
Example III using the following compositions.
Wt.
Component A B C D _ F
5 C14-15 alcohol
polyethoxylate (7)40.040.040.0 30.0 5.0 5.0
Sodium C13 linear
alkylbenzene
sulfonate - 10.0 5.0 5.0
20 Coconut alkyd
diethanolamide -I 0.5 0.5
C12-1~ fatty acid 5.6 5.65.6 5.6 --- ___
Sodium purify-
phosphate --- - 5.0 5.0
25 Sodium borax --- -I --- 2.0 2.0
Ethanol 3.0 3.0 3.03.0 --- ---
Diethylene glycol
monobutyl ether 12~0 12.012.0 12.0 --- ---
Propylene glycol10.010.0 10.010.0 --- ---
Triethanolamine 5.0 5.0 5.05.0 --- ---
Sodium car boxy-
methyl cellulose --- --- - - --- 0.5 0.5
Sodium hydroxide --- --- --- 0.02 0.59 0.59
Sodium 4-(2H-naphtho-
[1,2-d]triazol-
2-yl)-2-stilbene-
sulfonate 0.18 --- 0.120.18 1.0* ---

I 3

. .

- 34 -
Disodium Boyce-
((aniline-
methylhydroxyethyl-
amino-l,3,5-triazin-
2-yl)-amino)-2,2'-
stilbene disulfonate --- 0.18 0.06 --- -- lo
Water Balance to l00
*Brightener not in solution.
The results were as follows.
Grade - lo mender
Fabric A B C D E F
Coarse weave cotton lo 2.5 lo lo lo 3.0
Cotton sweater 2.0 3.0 3.0 T T 3.5
Unbleached muslin T 2.5 2.0 lo lo 2.0
Underwear T lo lo 0 0 lo
White T-shirt 0 0 0 0 0 T
Only Composition D is within the scope of the
present invention although the monosulfonated brightener
also provided reduced staining in A Which did not
contain an anionic surfactant) and E which was not a
stable isotropic liquid).
EXAMPLE XIII
Brightener staining was evaluated as described in
Example XI in the following composition.
25 Component Wt. %
Clue linear alkylbenzene sulfonic acid 7.2
Cl4_l5 alkyd polyethoxylate lo
sulfuric acid l0.8
Clue 13 alcohol polyethoxylate (6.5)S.5
on Cl2-l4 fatty acid l5.0
Citric acid (an hydrous) 4.6
Sodium diethylenetriamine pentaacetate 0.6
TAIPEI* 1.0
Monoethanolamine 7.0
35 Sodium hydroxide lo
Potassium hydroxide 0,94

:~L235S5~


Propylene glycol 4.0
Ethanol 6.5
Sodium format lo
Calcium hydroxide 0.15
Brightener As indicated
Minors and water Balance to 100
*Tetraethylene pentaimine ethoxylated with 15-18 moles
(avg.) of ethylene oxide at each hydrogen site.
Brightener
A = 0.12~ disodium 4,4'-bis~(4-anilino-6-methylhydroxy-
ethylamino-1,3,5-triazin-2-yl)amino)-2,2'-stilbenee
disulfonate + 0.06% disodium 2,2-(4,4l-biphenylene
divinylene)-dibenzenesulfonate
B = 0.18% sodium 4-(2H-naphtho[1,2-d] triazol-2-yl)-2-
stilbenesulfonate
C = 0~15~ sodium 4-(2H-naphtho[lJ2-d] triazol-2-yl)-2-
stilbenesulfonate + 0.02% disodium Boyce-
anilino-6-methylhydroxyethylamino-1,3,5-triazin-2--
yl)amino)-2,2'-stilbene disulfonate
D = 0.15% sodium 4-(2H-naphtho[1,2-d] triazol-2-yl)-2-
stilbenesulfonate 0.02% disodium 2,2-l4,4'-
biphenylene divinylene)-dibenzenesulfonate
E = 0.12% sodium 4-(2H-naphtho[1,2-d] triazol-2-yl)-2-
stilbenesulfonate + 0.06% disodium 2,2-(4,4'-
biphenylene divinylene)-dibenzenesulfonate
The results were as follows.
Fabric Composition Grade
10 mender overnight/damp
Coarse weave
cotton A 2.8 4.0
" B T 2.5
" C 2.0 2.9
" D 0.5 3.1
.. E 1.5 3.3


~s~s3


- 36
Cotton sweater A 2.7 4.0
" B T 2.7
" C 1.3 3.2
" D T 3.3
" E 0.5 3.3
Unbleached muslin A 2.0 3.0
" B T 2.0
" C 1.0 200
" D T 2.0
" E T 1.3
Underwear A 2.0 3.5
" B 0 2.2
" C T 1.8
" D T 1~5
" E T 1.0
White T-shirt A T 1.5
" B 0 T
" C 0 T
if D 0 0
" E 0 T
Unbxightened
cotton knit A 1.5 3.8
B T 2.4
C 0.8 3.0
D T 3.1
E 0.3 3.3
UnbrightPned
cotton knit A 2.0 3.8
(bleached) B 0 1.3
C T 1.1
D T 104
E 0.3 1.0
Compositions B, C, D and E of the present invention
caused less staining of the cotton fabrics.
WHAT IS CLAIMED IS-

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Administrative Status

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Administrative Status

Title Date
Forecasted Issue Date 1988-04-26
(22) Filed 1985-06-27
(45) Issued 1988-04-26
Expired 2005-06-27

Abandonment History

There is no abandonment history.

Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Application Fee $0.00 1985-06-27
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
THE PROCTER & GAMBLE COMPANY
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) 
Drawings 1993-08-05 1 17
Claims 1993-08-05 2 65
Abstract 1993-08-05 1 11
Cover Page 1993-08-05 1 17
Description 1993-08-05 36 1,078