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Patent 2055340 Summary

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(12) Patent Application: (11) CA 2055340
(54) English Title: CONCENTRATED LIQUID DETERGENT COMPOSITION CONTAINING ALKYL BENZENE SULFONATE AND MAGNESIUM
(54) French Title: COMPOSITION DETERGENTE LIQUIDE CONCENTREE QUI CONTIENT DU SULFONATE D'ALKYLBENZENE ET DU MAGNESIUM
Status: Dead
Bibliographic Data
(51) International Patent Classification (IPC):
  • C11D 1/22 (2006.01)
  • C11D 1/29 (2006.01)
  • C11D 1/37 (2006.01)
  • C11D 1/655 (2006.01)
  • C11D 1/75 (2006.01)
  • C11D 3/02 (2006.01)
  • C11D 3/32 (2006.01)
  • C11D 7/50 (2006.01)
  • C11D 17/00 (2006.01)
  • C11D 1/52 (2006.01)
(72) Inventors :
  • JAKUBICKI, GARY J. (United States of America)
  • WARSCHEWSKI, DIRK (United States of America)
(73) Owners :
  • COLGATE-PALMOLIVE (United States of America)
(71) Applicants :
(74) Agent: SMART & BIGGAR
(74) Associate agent:
(45) Issued:
(22) Filed Date: 1991-11-12
(41) Open to Public Inspection: 1992-05-22
Availability of licence: N/A
(25) Language of filing: English

Patent Cooperation Treaty (PCT): No

(30) Application Priority Data:
Application No. Country/Territory Date
616,496 United States of America 1990-11-21

Abstracts

English Abstract


CONCENTRATED LIQUID DETERGENT COMPOSITION
CONTAINING ALKYL BENZENE
SULFONATE AND MAGNESIUM

Abstract of the Disclosure
A concentrated light duty liquid detergent composition
is described. The composition, which offers superior grease
cutting and foam mileage, contains a surfactant mixture of
magnesium alkylbenzene sulfonate, alkyl ethoxy sulfate and
optionally, alkyl sulfate. The composition also contains a
magnesium ion source in an amount such that the molar ratio of
total magnesium ion to alkylbenzene sulfonate ranges from about
0.65:1.0 to 1.0:1Ø


Claims

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



What is Claimed Is:
Claim 1. A liquid dishwashing detergent composition
providing stable foaming characteristics and which is especially
effective in removing greasy soils, said composition comprising:
(A) from about 20 to about 70% by weight of a
surfactant system comprising
(a) from about 15 to about 35% by weight of the
magnesium salt of a C10-C18 alkylbenzene sulfonic acid anionic
surfactant;
(b) from about 1 to about 5% by weight of a water
soluble magnesium salt, in an amount such that the molar ratio of
total magnesium ion to alkylbenzene sulfonate ranges from about
0.65:1.0 to 1.0:1.0,
(c) from about 1 to about 20% by weight of a
water-soluble C1-C16 primary alkyl ethoxy sulfate containing an
average of from about 1 to about 6 ethylene oxide groups per
alkyl group in the alkyl ether sulfate, and
(d) from about 0 to about 20% by weight of a
primary, secondary or tertiary amine or alkali metal salt of
C10-C18 alkyl sulfate; and
(B) from about 0.5 to about 8% by weight of a suds
promoting agent selected from the group consisting of C10-C18
ethoxylated and non-ethoxylated mono- or di- C1-C5 alkanolamides
and C12-C14 alkyl amides condensed with up to about 15 moles
ethylene oxide per mole of amide;
(C) from about 0 to about 10% by weight of a low
irritant organic solvent;
(D) from about 0 to about 10% by weight hydrotrope; and
(E) from about 0 to about 10% by weight of one or more
optional additive chosen from chelating agents, coloring agents,




dyes, perfumes, bactericides, fungicides, preservatives,
sunscreening agents, pH modifiers, pH buffering agents,
opacifiers, antioxidants, proteins and
(F) the balance, water.
Claim 2. The composition of Claim 1 that comprises
(A) from about 30 to 55%;
(B) from about 1 to 6%;
(C) from about 5 to 8%;
(D) from about 0 to 6%;
(E) from 0 to about 3%; and
(F) the balance, water.
Claim 3. The composition of Claim 1 wherein the
surfactant system (A) comprises (a) from about 19 to 21% by
weight of a magnesium salt of a C10-C18 alkylbenzene sulfonic
acid; (b) an amount of a water-soluble magnesium salt such that
the molar ratio of magnesium ion to alkylbenzene sulfonate is
0.65:1.0 to 0.8:1.0; (c) from about 10 to about 13% by weight of
a C10-C16 alkyl ethoxy sulfate with 3 groups of ethylene oxide
per mole of alcohol; and (d) from about 10 to about 15% by weight
of a C10-C16 alkyl sulfate.
Claim 4. A physically stable liquid dishwashing
detergent bass composition comprising:
(A) from about 30 to about 70% by weight detersive
active ingredients comprising
(a) from about 10 to about 50% by weight of the
magnesium salt of a C10-C18 alkylbenzene sulfonite acid;
(b) from about 1 to about 5% by weight of a water-
soluble magnesium salt, in an amount such that the molar ratio of
total magnesium ion to alkylbenzene sulfonate ranges from about
0.65:1.0 to 1.0:1.0;

21


(c) from about 1 to about 27% by weight of a
water-soluble C10-C16 primary alkyl ethoxy sulfate salt
containing an average of from about 1 to about 6 ethylene oxide
groups per alkyl group;
(d) from about 0 to about 27% by weight of a
primary amine or alkali metal salt of a C10-C16 alkyl sulfate;
and
(B) from about 0.6 to about 11% by weight of a suds
promoting agent selected from the group consisting of a C10-C16
mono- and di-C1-C5 alkanolamides and C12-C14 alkyl amides
condensed with up to 15 moles ethylene oxide per mole of amide;
(C) from about 0 to about 10% by weight of a low
irritant organic solvent;
(D) from about 0 to about 8% by weight of a hydrotrope;
and
(E) the balance, water.
Claim 5. The composition of Claim 4 that comprises:
(A) from about 60 to 65%;
(B) from about 1 to about 8%;
(C) from about 2.5 to about 3.5%;
(D) from about 1 to about 5%; and
(E) the balance, water.
Claim 6. The composition of Claim 4 wherein the
surfactant system (A) comprises a water-soluble magnesium salt in
an amount sufficient to provide a molar ratio of total magesium
ion to magnesium alkylbenzene sulfonate in the range of 0.65:1.0
to 0.8:1Ø


22

Description

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


l ~ 2~3l~


CONCENTR~TED LIQUID D~T~RG~NT COMPOSITION
CO~T~I~ING ALXYL BFNZBNF
¦ SULFONA~E AND MAGN~SIUM

BACKGROUND OF THE INVENTION
Fileld Of Tlle Invention:
This invention relates to aqueou~ liquid detergent
compositions containing alkyl benzene sulfonate and added
detergent boosting levels of magnesium ion~.
Description Of The Prior Art:
Light-duty liquid detergent compo~itions, such as those
Ruitable for uRe in washing di~he~, are well known. Performance
of such compositions is a measurement of both foam mileage, i.e.
number of dishe~ washed, and grease cutting ability. The liquid
dishwashing detergent compo~itions pre~ently on the market are
designed to remove oily/grea~y ~oils from glasses, dishes, and
other tableware and kitchen uten~ils while maintaining an
acceptable layer of ~uds.
Liquid detergent formulations containing magne~ium
salts and magnesium surfactant~ show enhanced performance, a~ i8
disclosed in U.S. Patents 2,908,651 and 2,437,253. Certain
combinations of active ingredients can also provide a range of
enhanced detergent properties. An enhanced performance liquid
detergent compo~ition, discloHed in U.S. Patent 4,435,317,
contains (a) a Clo-cl6 alkyl sulfate~ (b) a C10-C16 alkyl ethoxy
sulfate and (c) a linear Clo-C16 alkyl benzene ~ulfonate in a
ratio of the total weight of (a) + ~b) to the weight of ~c) of
le88 than or equal to 33:1, and containing magne~ium in a molar
amount corresponding to 0.20x-0.70x where x is the number of
moles of alkyl sulfate. The amount of magne~ium salts that can
be added to the compositions di~clo~ed in U.S. Patent 4,435,317

I 2~sr s3~



is limited because the salts raise the temperatures at which
inorganic salt crystal~ ~orm in the composition~ upon cooling.
Enhanced performance in relation to grea~e cutting
a~ility and foam mileage are al~o achieved by increasing the
concentration of surfactant active ingredients in the liquid
detergent formulation. There are, however, several problem~
associated with the preparation of liquid detergent compositions
cdntaining high proportions of active detergent materials in
order to ~ati~fy the requirements of clarity, vi8c08ity and
stability of the product.
Generally, it is necessary to add a fairly high
proportion of hydrotrope to those detergent compositions that
have a high concentration o active detergent materials.
Hydrotropes are fairly expensive and are generally inactive
material~ and thus do not contribute to detergency but have the
effect of rendering the active ingredients water soluble and the
compo~ition homogeneous at those temperatures normally
encountered in transport and storage. Hydrotropes generally
lower the "cloud poi~t" of liquid detergent compositions, thus
maintaining a clear liquid composition at temperatures at which a
detergent composition lacking hydrotrope would become cloudy and
unattractive in appearance. U.S. Patent 4,235,758 discloseR that
t~e use of a magnesium alkylbenzene sulfonate derived from a
linear Clo-C13 alkyl~enzene of average molecular weight of 220-

250 significantly reduces the requirement for hydrotrope at anylevel of active detergent material.
The present invention provides compositions comprised
of certain specific detergent active ingredients, in unique
combinations and proportions, whlch are unexpectedly capable of


~ ~,! 2 ~ ~ ~ 3 i~ ~

~uperior performance to other liquid detergent~ in relation to
both foam mileage and grease ~utting.
It i~, accordingly, an ob~ect of thi~ invention to
provide physically stable liquid detergent compositions that
offer superior grea~e cutting and foam mileage performance.
It is another object of this invention to provide
detergent compositions containing magne~ium, alkylbenzene
sulfonate and added detergency boosting level~ of magne~ium ions,
which are e~pecially efficient in removing grea~y 80il8, and
which have a reduced requirement for hydrotrope~ to maintain a
suitable cloud point.
Still another object of this invention is to provide a
concentrated detergent ba~e compo~ition containing detergency
boo~ting level~ of magne6ium ions and alkyl benzene sulfonate
which may be stored a~ a concentrated liquid base composition and
which may be manufactured using conventional low shear liquid
mixing equipment.
SUMMARY OF THE INVENTION
According to the present invention, there is provided
an aqueous liquid detergent composition e~peaially suitable for
~-se in dishwa~hing, and containing
(A) from 20 to 70~, preferably 30 to 55%, of a
. ~urfactant mixture of (a) from about 15 to about 35~ by weight
of the magnesium salt of a Clo-Clg alkylbenzene ~ulfonic acid,
~b) from about 1 to 5% by weight of a magnes1um salt, in an
amount such thut the molar ratio of total magne~ium ion to
alkylbenzene sulfonate ranges from about 0.65~1.0 to 1.0:1.0, (c)
from about 1 to about 20% by weight of a water-soluble Clo-C16
primary alkyl ethoxy sulfate containing an average of from about
1 to 6 ethylene oxide groups per alkyl group in the alkyl ether




: :..', . . . -,. ':, -: '
.. . ..

2~3~ ~

sulfate and, (d) from about o to 20% by weight of a primary,
~econdary or tertiary amine or alkali metal salt of C10-Cl6 alkyl
~ulfate; and
(B) from about 0.5 to about 8% by weight of a ~ud~
promoting agent selected from the group consi~ting of C10-Cl8
ethoxylated and non-ethoxylated mono- or di- Cl-C5 alkanolamide~ :
and C12-C14 alkyl amides condensed with up to about 15 mole~
ethylene oxide per mole of amide, and balance, primarily water.
In a preferred embodiment the composition may also
include:
~ C) from about O to about 10% by weight of a low
irritant organic solvent; and
(D~ from about O to about lO~i by weight of a
hydrotrope. The compositions may also include
(~) other adjuvants, such as chelating agents, coloring
agents, dyes, perfumes, bactericide~, fungicides, preservative~,
sunscreening agents, pH modifiers or buffering agents,
opacifier~, antioxidants, proteins, and the like.
The present invention also provides a pourable liquid
detergent ba~e composition of concentrated light duty liquid
detergents containing alkylbenzene sulfonic acid and detergency
boosting levels of magnesium ions and which can be stored at
ambient temperature for future use without gelling.



DET~ILED DESCRIPTION OF T~E INVENTION
Detergent compositions ~n accordance with the present
invention comprise a mixture of two or three es~entlal anionia
surfactant3 of defined constitution and proportions and have a
pecified molar ratio of magnesium ion to alkylbenzene sulfonate


ranging from 0.65:1.0 to l.Osl.O.
.




:' '.' ' :' ' ' ,'., . ' ' ',:'....... '"':. , , :
. :. ,.. , . ~ ; :

~ r~



The first essential surfactant ingredient i~ a water-
soluble salt of alkylbenzene sulfonic acid, which may be linear
or branched. The alkyl group preferably contain~ from about 10
to 18 carbon atoms, mo~t preferably from about 11 to 13,
especially about 12 carbon atoms, pr~ferably in a linear chain
configuration. The alkyl benzene sulfonate may ~e present a~ an
alkali metal, amine, ammonium, or alkaline earth metal ~alt,
preferably the ma~nesium salt. Thu~, the most preferred
alkylbenzene sulfonate i8 the magnesium ~alt of linear
dodecylbenzene 6ul fonate.
The acid form of alkylbenzene ~ulfonic acid can be
converted to the magne~ium salt form either prior to admixture
with the other detersive ingredient~ or thereafter. The
conver~ion may be accomplished either by direct neutralization
with magnesium oxide or hydroxide or by ion exchange between, for
example, an alkali metal salt or the ammonium salt of
alkylbenzene ~ulfonate and a water-soluble alkaline earth metal
salt. Preferably, a source of magnesium ions i~ added to the
detergent mixture to form the de~ired ~alt of alkylbenzene
sulfonate. Magnesium chlorides, magnesium sulfate~, magnesium
acetates or magnesium hydrGxides are examples of magnes3um
sources. ~he preferred magnesium eources are magne~ium oxide~
or hydroxide~ and sulfates.
The alkylbenzene sulfonate component 3 8 present at a
level of from about lS to 3S% by wffight of the composition,
preferably in the range from about 15 to 22~, mo~t preferably in
the range from about 19 to 21% by welght.
The point of attachment of the alkyl chain to the
benzene nucleus, referred to as the phenyl isomer distribution,


' 2~3~

8 not critical but, preferably, les~ than 20% of the alkyl
benzene of this invention comprises the 2~phenyl i~omer.
A second essential surfactant component of the present
1 omposition is a primary alkyl ethoxy sulfate derived from the
¦ ondensation product of a C1o-C16 alcohol with an average of
rom about 1 to about 6 ethylene oxide groups, preferably about 2
to 4, especially 3 ethylene oxide groups per mole of alcohol.
The C10-C16 alcohols may be derived, for example, from natural
fats or Ziegler olefin build-up or Oxo ~ynthesis. It i8
preferable to use alkyl ethoxy sulfates and alkyl sulfates of the
same carbon chain length, preferably C12-C13. The level of
alkyl ethoxy ~ulfate in the present composition to achieve the
desired foam and deterRive propertie~ is about 1-30% by weight,
preferably in the range from about 10-20~ by weight, based on the
total compo~ition.
The surfactant system of the detergent of the present
invention may optionally also include an amount ranging from
0-20% of the total composition, preferably 10-15~ by weight, of
an alkali metal or ammonium or amine salt of a linear or branched
Clo-Clg alkyl sulfate anionic surfa¢tant. The cationic counter-
ion of the alkyl sulfate may be taken from the group consi~ting
of alkali metals, ammonia and amines, e.g., triethylammonium,
tr,iethanolamine ~TEA), diethanolamine or monoethanolamine, etc.
The alkali metal may be, for example, sodium or potassium, ~:
preferably sodium.
The composition of the present invent~on contains from
about O.Q27 to about 0.064 moles of total magnesium ion.
Generally, 0.023 to about 0.053 moles of magnesium ~on are
provided through the incorporation of the magne~ium alkylbenzene
sulfonate. Additional magnesium may be added to the composition




' : ',.', . '. ' .; . ' ' - : .. ' :.- '' '

~ 2 ~ 5 ~ J


in the form o~ a water-soluble compound, mo~t pre~erably a salt,
such as, for example, magne3ium Rulfate or magne~ium chloride.
The preferred magne~ium ~ource i8 magneBium ~ulfate heptahydrate,
added to the composition at about from 1 or 2 to 5% by weight,
preferably from about 2.5 to 3.5% by weight, corre~ponding to
0.01 to 0.014 moles of added magnesium. The total magne~ium ion
to alkylbenzene sulfonate in the composition i8 aontrolled to
correspond to a molar ratio of from 0.65:1.0 to 1.0:1.0,
preferably from 0.65:1.0 to 0.8:1Ø
The additional magnesium ion~ addet in ~alt form
provide improved grease cutting performance and also lower the
cloud point of the formula better than the more expensive
hydrotropes. The additional magnesium ~alt also provides better
phase stability to the composition. Uning magnenium to boost
lS detergency is known in the art, however, when used in a molar
ratio of total magnesium ion to alkylbenzene sulfonate in a range
of 0.65:1.0 to 0.8:1.0, the exce~s magnesium salt not only
enhances foam mileage but al~o increases fluidity, allowing for a
decrease in hydrotrope and alcohol levels, thus lowering the
concentration of inactive ingredients that do not boost
detergency of the composition. This decrea~e in the level of
inactive ingredients leaves room in the composition for an even
higher level of detersive active ingredients.
The level of detersive active ~ngredients in the
compositions of this inv~ntion ia in the range from 20-70% by
weight, preferably from 30 to 55%. This increased level of
aqtive ingredients results in enhanced foam mileage, thus
providing a superior light duty liquid detergent. The usual
problems of increased viscosity, decreased stability and product
clouding is avoided by using an increased level of magnesium ions




: ;. . , . , ' . ',' ,,:, . .
'-'' ~ '.'' . . , .'' .' . ' ' '; ' '' '.','' ",' '

2 0 a ~ ,f~

fn a molar rati~ of magnesium ions to alkylbenzene sulfonate in
the range of 0.65:1.0 to 1.0:1.0, preferably from to 0.8:1.0 and
none or only a low concentration of hydrotrope. The additional
magnesium ions in the compositions of this invention also boost~
detergency of the surfactant system.
In general, the consumer views sudsing ab~lity a~ a
measure of cleaning ability. A suds promoting agent, such a~,
for example, a mono- or di-alkanolamide, may, therefore, be added
to the present composition at a level of from 0.5 to about 8~ by
10 weight, preferably about 1 to 6% and, more preferably about 1 to
5% by weight. The preferred suds promoting agent i8 a mixture of
lauric and myristic monoethanolamides. Alternatively, the alkyl
~roup of the amide may be derived from coconut or palm kernel
oil. Suitable alkanolamides include either mono or
15 dialkanolamides having a carbon chain distribution of Cl-Cs,
preferably C1-C3, especially mono- or di-ethanolamide. The
alkanolamide may be ethoxylated or may be a mixture of non-
ethoxylated alkanolamide and ethoxylated alkanolamide in order to
increase the solubility of the alkanolamide in the composition~
~lthough not essential, clarity and homogeneity of the
invention compositions may be improved by inclusion of, for
example, organic solvents or hydrotrope~ and these and other non-
essential additives may be included in the compo~itions in
amounts that do not adver~ely effect the desired properties.
25 Organic solvents may be included for their thinning effect,
ability to lower the clear point and for solubilization.
Organic solvent~, ~uch as, for example i~opropanol, n-propanol,
ethanol, propylene glycol or mixtures thereof may be included.
When used, the solvent level iB u~ually les~ than or equal to 10%
30 by weight, preferably less than 8~, more prefer~bly ln the range
' 8




' ' '. , !' . ' . : ' . . .

2~55~'~u


of 5 to 8% by weight. Ethanol i8 the preferred solvent. It i~
also cu~tomary to include a hydrotropic ~ubstance in the
composition such a~, for example, urea, ~odium xylene sulfonate,
potassium xylene ~ulfonate, sodium cumene sulfonate, and ammonium
x~lene sulfonate, and the like in order to a~sist in
solubilizing various components of the composition and
maintaining a low clear point. Mixture~ of two or more
hydrotropes may also be used. The hydrotrope, when used, is
generally present in amounts below 8%, preferably below 6%, such
as 1 to 6%, especially 2 to 5~ by weight.
Various other optional ingredient~ may also be included
in the composition for their de~irable a~sthQtic or functional
characteristics. Such ingredients include, for example,
opacifying agents to make the composition appear pearly, such as
behenic acid or ethylene glycol distearate; perfumes; heavy metal
chelating agents such as EDTA; bactericide~ such as
trichlorocarbanilide, tstrachloro~alicylanilide,
hexachlorophene, or chlorobromo~alicylanilide; antioxidants;
thickeners such as guar gum, polyacrylates, polyacrylamide or
I~i~h mo~s; dyes, water dispersible pigments; preservative~, such
as formaldehyde or hydrogen peroxide; pH modifiers, etc. When
u~ed, these optional adjuvants may be present in total amounts up
to about 10~ by weight, preferably up to about 3~ by weight,
based on the total compo~ition. The pH o~ the compositions mny
be within the range from 6 to 8, preferably from about 6.5 to
7.5, and may be adjusted if nece~sary by add~tion of suitable
acids or bases, such as HCll NaOH, and the l~ke. ~xcellent
greasy soil removal i8 attained when an effective amount of the
instant compositions is di~olved in an aqueous dishwa~hinq
~olu~ion. Typical use concentrations are usually at least about




""'.-'.' ' ' ' ' - ' " ' ' - . .: ' . '' . ' '.,.':,.. ,' '

2 ~3 3 ,~

0.05~ by weight in water. of cour~e, thi~ can be adju~ted,
depending on the soil level and type and desires of the user.
Currently, great commercial interest is ~hown in the
more concentrated liquid detergent compositions. The advantages
of highly concentrated liquids are evident, i.e., reduced
transport and packaging costs and smaller quantitie~ of product
needed by the consumer. The major disadvantage in developing
compositions with high active ingredient levels i8 the difficulty
in making the ~ormula due to the increased "solids"
concentrations. The word "solid~" is used herein to describe all
those ingredients of the composition other than solvents, such as
water or alcohol.
The compositions of the present invention employ high
levels of anionic surfactants, which are, in general, less
water-soluble than nonionic surfactants. The decreased
solubility of the anionic ~urfactants coupled with the increased
concentration of active lngredients often results in thick paste~
with very high viscosities, thereby necessitating the use of
heavy duty or high shear mixing equipment. Accordingly, in a
preferred mode for carrying out the present invention a non-
conventional process is used for the manufacture of the
compogition~ of the present invention.
According to this preferred method, a detergent ba~e
comprising magnesium alkylbenzene sulfonate and amide foam
2S booster is preferably manufactured by a proce0~ wherein
alkanolamide, in the specified amount, is added to an aqueous
slurry containing magnesium oxide or hydroxide, hydrotropes, and
any inorganic salts or organic solvents of the liquid detergent
compositions of this invention, in the speoified amounts, and the
alkylbenzene sulfonic acid, i8 added after the alkanolamide has




:: . . .. .: . :.
' ." ' . ,'' . ,' . ' ,.: '. ' ' ' " ' . , ' . "' . ' . ,' ' " : ' " "' ' ' : '

~ ~ 2 ~


been dissolved in the slurry. This procedure i~ de~cribed in
greater detail in our copending application Serial No. _ ,
filed on the same date as the subject application under
attorney~ docket IR-4863, titled "PROCESS FOR PRODUCING
CONCENT~ATED LIQUID DETERGENT BASE CONTAININ& MAGNESIUM
ALKYLBENZENE SULFONATE AND ALKANOLAMIDE", the disclo~ure of
which iB incorporated herein in its entirety by reference
thereto. This method has the advantage of utilizing conventional
liquids mixing equipment, while resulting in a composition with
enhanced fluidity during neutralization and upon cooling.
The following representative non-limiting examples
will illustrate the invention although applicants do not intend
td be bound thereby.


2~5~3~

Example 1.
' The following composition~ are prepared with
conventional low shear mixing equip~tent by mixing the materials
in the proportion~ as listed.



Run No.

(Wt.~)
Water, deionized 11.66 11.28
TEA lauryl sulfate (40% solution)28.75 - 28.75

Sodium alkyl ethoxy
sulfate, 3E0 18.02(66.6S) 17.7(67.8%)
Sodium xylene sulfonate (40% 801.) - 5.23
Sodium cumene sulfonate (93%~ 2.9 1.0
Magnesium oxide 1.16 1.16
l gS04 7H20 1.0 3.0

a,2S4 1.5 0.5
auric/myri~tic monoethanolamide(prill) - 3.49
Lauric/myristic monoethanolamide~sodium
ylene ~ulfonate 5:3 blend 8.72 -
thanol 5.5 7.5
Dodecylbetnzene sulfonic acid 18.75 18.87
Minor ingr~dients ~dye, perfume, etc.) 2.04 1.5
100% 100~
Molar ratio of Mg+2: Alkylbenzene 0.54sl.0 0.67sl.0 s
sulfonate s
Cloud point 6C 0C




The compo~ition of Run No. 2 is a physically stable
liquid upon accelerated aging at elevated temperature. The
composition of Run No. 1, while having a higher hydrotrope level,
, 12




. : . . .,. , ... . ....

2~3~3~

was found to exhibit pha~e separation on aging~ Eaah of the
compositiOns of Run~ 1 and 2 ar~ ~valuated by the following
perEormance criteria:
(1) Grease Removal Test
This te~t is used to measure grease removal of the
composition at a concentration of 1% liquid detergent a~ 50 ppm
water hardness, at 80F, with 600 dipping cycle~ at 60 rpm. For
this te~t, 0.5 grams of lard at room temperature is evenly
applied to a frosted gla~s micro~cope slide using a ~errated
knife blade. The re~ults are calculated as milligrams of lard
removed.
A modified version of-the Grea~e Removal test is uced
to measure grea~e removal of a 0.05% solution of liquid detergent
at 50 ppm water hardness and lQ8F, with 600 dipping cycles at
60 rpm. For this test, 0.1 + 0.02 grams of lard is applied to
plastic test tubes by d~pping the pre-weighed tube~ in melted
lard and blotting off any exces~ grease before it solidifies.
The tubes are then re-weighed and used the same day they are
prepared.
Detergent compositions to be tested are prepared,
warmed to the appropriate temperature and poured into 250 ml
beakers. The de3ired temperature of the Bolution i8 maintained
by a circulating water bath. The teBt compoBition iH agitated
with a stirring rod until a layer of foam covers the top of each.
The beakers and ~oiled tubes are placed in the dipping apparatus
which iB then run at 600 cycles at 60 rpm. Upon completion of
the te~t cycle, the tub2s are removed, rinsed in deionized water
at 77F, air dried overnight and weighed. The ~oil removal
performance (percent cleaned) iB then calculated by the following
formula:




"" '"''' i'''' '' " ' '''"' '';''''''' '''' ' ''' '"'' ;"" ''''"' '
"'' ' '' .' .' '~',' . ;':: -, ';,'. '-' ' ,;. ;'.), -


20a53 ~


% cleaned = _ x 100,B-A
l where A = the weight of the tube, B ~ the weight of the
¦ tube plus soil, C = the weight of the tube after washing.
comparison of the average amount of greasy 80il
removed by the composition of Run No. 2 with a be~t selling light
duty dishwashing composition (Control 2) as determined by the
l Grease Removal test at 0.05~ detergent concentration, 50 ppm
¦ water hardne~, 108F, 600 dipping cycle~ at 60 rpm is ~hown in
l Table 1.
¦ (~) Hand Disll Washing Test
Six liters of a diluted (0.1% or 0.075%) test solution
l prepared using 50 ppm water at 120F is delivered to a dish pan
¦ from a separatory funnel suspended above the pan to generate a
layer of foam. Plates soiled with 5.4 grams lard are washed to a
foam end point. This test measures the total number of plates
that can be wa~hed with the detergent composition until ths foam
completely disappear6.
~C) Dynamic Yoam Stability Test:
This test i8 used to determine the dynamic foam
stability of a liguid detergent composit~on at 50 ppm water
hardness at 113P.
A diluted ~0.05 or 0.04%) test ~olution i8 titrated
with constant delivery of mixed ~oil to a foam end point under
constant agitation. The test mea~ures the amount of mixed soil
reguired to deplete the sur~actants of the composition.
~D) Cylinder Foam Test:
I This te~t i~ used to determine ths Eudsing ability of a
liquid detergent composition at 50 ppm water hardness at 113F.

100 mls of a 0.1% LOL test solution is placed in a
500 ml graduated cylinder. The cylinder i~ inverted 20 time~
and the amount of foam i5 meanured. Soil (0.01 gram~ added
to the solution and the cylinder is again inverted 20 times. The
decrease in foam level is then noted.
The resultg of the testing for the compo~ition~ of Run
Nos. 1 and 2 and the re~ult~ of two different be~t selling
commercial light duty di~hwasher compositions are ~hown in
Table 2.


~53~

TABLE 1
,Averaqe Soil Removal
108F
Run 2 50.9
Control 2 22.1



The resultB of this test indicate that the composition
of Run No- 2 removes twicQ a~ much greasy ~oil at 108F than doe~
a leading commercial brand of hand dishwashing detergent
containing ~imilar dQtersive active ingredionts but which has a
molar ratio of magnesium ion to alkylbenzene sulfonate of
0.31:1Ø


~ 5~

TABLE 2

Performance Te~t~-Set I Performance Te~ts-set II
Test Method Run. 1 Control 1 Ratio Run 2 Control 2 Ratio

Hand Dish (1) 34.5 28.51.21 - - - - - - - - - -
0.1% LDL
5.4g lard
120 F
Hand Dish (1) - - - - - - - - - - 35-7 33-4 1~07
0.075% LDL
5.4g lard
120 F
Grease Removal(2) 107 40 2.68 220 190 1.16
1% LDL
600 cycles
60 rpm
lard ~oil
80F
Dynamic Foam
Stability Test~31 1.21 1.09 1.11 1.37 1.28 1.07
113 F
Cvlinder Foam ~4~ 375/ 205/ 1.83/ 365/ 285/ 1.28/
0.1% LDL 342 165 2.07 335 265 1.26
20 cycles
30 rpm
100 F
(0.01 mixed food 80il )
All tests use 50 ppm hardness water.
(1) Hand dish results are in plate count to foam end point.
(2) Grease Removal results are milligrams of lard removed.
t3) Dynamic Fo~m Stability results are foam performance ratio~
versus a standard liquid detergent composition containinq 34%
surfactant ingredients.
~4) Cyl;nder test results are CC~8 of foam (no soil/with soil)-




' ,''; - - '. ~ . ., ~ -.'............................ :.
.. .. . ..

2 ~ ~ 5 3 ~ ~

Control 1: Leading commercial brand of hand dishwa~hing
~omposition containing 50% active ingxedients
including 17% linear alkylbenzene sulfonate, 23%
alkyl ethoxy sulfate, 10% fatty acid mono-
S ethanolamide and a total magnesium content of 0.70% .
~his composition has a molar ratio of magnesium to
alkylbenzene sulfonate of 0.58:1Ø
Control 2: A second leading commercial brand of hand
di~hwashing composition containing 56% active
~ ingredients including 24% linear alkyl benzene
sulfonate, 22~ alkyl ethoxy ~ulfato-3EO, 10%
ethoxylated fatty acid monoethanolamide and also
containing 0.5% magnesium, corresponding to a molar
ratio of magnesium to alkylbenzene sulfonate of
0.31:1Ø




18




, .,, ~ . ...... , ,, ,.,; ,,, , . . , ; ,, , . ;, ;, . . .

~;3~3'~

Exam~le 2.
A stable pourable liquid detergent composition i~
prepared by mixing the following ingredient~ u8ing ~ conventional
low shear liquids mixing apparatu~. The proportion of each
ingredient i8 a8 follows:


~ lWt-~Z
Water, deionized 22.1 17.6
~EA lauryl ~ulfate - 12.0
Sodium alkyl ethoxy ~ulfate 3E0 14.0 15.2
Sodium xylene sulfonate (40% 801) 12.0 13.1
S~dium cumene sulfonate (45% ~ol.) 4.7 5.2
Magnesium oxide 1.8 1.1
MgS04-7H20 4.8 5.5
Na2S4 ~ 0~5
Lauric/myristic monoethanolamide (prill) 8.0 8.0
Propylene glycol 2.3 2.5
Dodecylbenzene sulfonic acid30.3 19.3
Total 100 100
Consistency at 25C Physically Phy~ically
stable stable
l~quid l~quld




-, -, , , - .. , . : ...... . .

. .. - : . : . . :. . : -

Representative Drawing

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Administrative Status

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Administrative Status

Title Date
Forecasted Issue Date Unavailable
(22) Filed 1991-11-12
(41) Open to Public Inspection 1992-05-22
Dead Application 1999-11-12

Abandonment History

Abandonment Date Reason Reinstatement Date
1998-11-12 FAILURE TO PAY APPLICATION MAINTENANCE FEE
1998-11-12 FAILURE TO REQUEST EXAMINATION

Payment History

Fee Type Anniversary Year Due Date Amount Paid Paid Date
Application Fee $0.00 1991-11-12
Registration of a document - section 124 $0.00 1992-06-10
Maintenance Fee - Application - New Act 2 1993-11-12 $100.00 1993-01-27
Maintenance Fee - Application - New Act 3 1994-11-14 $100.00 1994-10-18
Maintenance Fee - Application - New Act 4 1995-11-13 $100.00 1995-10-16
Maintenance Fee - Application - New Act 5 1996-11-12 $150.00 1996-10-16
Maintenance Fee - Application - New Act 6 1997-11-12 $150.00 1997-10-17
Owners on Record

Note: Records showing the ownership history in alphabetical order.

Current Owners on Record
COLGATE-PALMOLIVE
Past Owners on Record
JAKUBICKI, GARY J.
WARSCHEWSKI, DIRK
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) 
Cover Page 1992-05-22 1 17
Abstract 1992-05-22 1 23
Claims 1992-05-22 3 113
Drawings 1992-05-22 1 7
Description 1992-05-22 19 713
Fees 1996-10-16 1 71
Fees 1995-10-16 1 60
Fees 1994-10-18 1 60
Fees 1993-01-27 2 119