Title of Invention

METHOD FOR IMPROVING SOFTNESS AND WRINKLE REDUCTION OF FABRICS

Abstract A method for treating a fabric comprising, in no particular order, the steps of: (a) contacting a hydroxy comprising fabric with at least one combination or compound selected from the group consisting of a first compound and a second compound, the first compound and a third compound, the second compound and the third compound; and the second compound; and (b) allowing the first and the second compound to react with a hydroxy group of the fabric, or (c) allowing the first or the second compound to react with a hydroxy group of the fabric and the third compound to react with the first or second compound, or (d) allowing the second compound to react with a hydroxy group of the fabric, or (e) allowing any combination of steps (b) to (d); wherein the first compound is a polycarboxylic acid, the second composition is a reactive functionalized siloxane and the third compound is a silicone compound containing a hydroxy group, a silanol group, or another functional group that can react with the first compound or the second compound.
Full Text FORM2
THE PATENTS ACT, 1970 (39 of 1970)
COMPLETE SPECIFICATION (See section 10; rule 13)

1. Title of the invention
2. Applicant

METHOD FOR IMPROVING SOFTNESS AND WRINKLE REDUCTION OF FABRICS
(a) Hindustan Lever Limited
(b) ofHindustan Lever House, 165/166, Backbay Reclamation, Mumbai 400 020, Maharashtra.
(c) an Indian Company ;

The following specification (particularly) describes the nature of this invention (and the manner in which it is to be performed)

METHOD FOR IMPROVING SOFTNESS AND WRINKLE REDUCTION OF FABRICS
FIELD
The present disclosure relates to laundry product compositions that provide substrates, such as fabrics, with durable Wrinkle reduction benefits and with improved softness. The composition can be used in both domestic and industrial processes.
BACKGROUND
Durable press treatments (a.k.a. "permanent" press 'treatments) in the textile industry are well known. In the 1960's, it was known .to use polycarboxylic acids for permanent press treatment of textiles. Generally, cellulose fibre can be cross-linked and esterified with polycarboxylic acids, particularly those with two or more carboxylic acid groups . Esterif ication is achieved upon heating the treated cellulose fibres _such_as_by ironing or other from of treat pressing. Curing catalysts, such as phosphorous containing salts, are also known and serve to aid cross-linking. The

treated arid cured textile is generally strengthened and is less likely to wrinkle during use. Examples of US patents relating to durable press finishing of cotton textile with polycarboxylic acids include: 4,820,307 (Welch et al.j, 4,975,209 (Welch et'al.) and 5,221,285 (Andrews et al.). The contents of these patents are incorporated by reference.
A disadvantage of known durable press treatments is . that the treated and cured textile is typically less soft as compared to the uncured textile. In order to increase softness, inert nonionic or anionic materials have been proposed in formulations as fabric softeners. These softeners include polyethylene, polypropylene and silicone softeners. A disadvantage of these softeners is that they require an additional treatment step subsequent to the durable press treatment and are not durable.
Therefore, there is a need for durable press treatments that not only impart wrinkle reduction benefits but also impart softness benefits, i.e.; durable softness. It would be preferable of the softness, benefits could be achieved without additional "steps subsequent to the durable press treatment.

SUMMARY
The present disclosure relates to durable wrinkle reduction products that impart durable softness. The products can be any substrate that have hydroxyl groups capable of forming cross-linked matrices. If the substrate is a fabric, the softness benefits are realised, for example, after machine or line drying.
In a preferred embodiment, silicone containing compounds are incorporated into the cross-linked matrix of cellulosic fibres of fabric. This is achieved by other 1) reacting the hydroxyl groups of the cellulosic fibres with polycarboxylic acids, wherein the polycarboxylic acids have silicone containing molecules and/or 2) by reacting, other molecules having both hydroxyl groups.and one or more silicones with the cross-linked polycarboxylic acid/cellulose- matrix. It is believed that the incorporated silicone molecules will provide lubrication of the fibre surfaces, resulting in wrinkle reduction, softening and less abrasion on the fibre surface. A most preferred embodiment includes silicone carboxylates, however any silicone compound containing a hydroxy or silanol group or other

functional group that cah react with the cross-linked.matrix can provide the desired affect. When cured to form an ester, the silicone containing molecules are difficult to remove under normal wash and wear conditions.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Durable press treatment of cellulosic fibres is achieved by the esterification of cellulosic hydroxyl groups with polycarboxylic acids. The present disclosure of durable softness is achieved by including silicone carboxylates into the formulations. Silanols and hydroxy containing organically modified silicone fluids can be incorporated into the cross-linked matrix by reacting with (i.e. another esterification reaction) with the polycarboxylic acid.
Other molecules containing multiple hydroxyl groups, such as triethanol amine, can be incorporated into the cross-linked matrix. The silicone carboxylates could also react with these molecules.

The durable softness compounds are preferably selected from the following molecular classes : silicon carboxylates; silanol fluids; silanols and hydroxy containing organically modified silicone fluids. Most preferred compounds are coarboxylic acid derivatized silicones that include any silicone with a -COOH group. These compounds are preferably incorporated into formulations useful for forming cross-linked matrices with cellulosic fibres. Preferred compounds for forming cross-linked matrices include, for examples, 1, 2, 3, 4 cyclopentanetetracarboxylic acid, 1, 2, 3, 4 butanetetracarboxylic acid (BTCA) and polyacrylic acids. Other suitable carboxylic acids are disclosed in the above-cited patents and in U.S. Patent 5,965,517 (Mooney), the contents of which are incorporated herein by reference.
A highly preferred composition in accordance with the present disclosure is Monosil® PCA (polysiloxyl pyrrolidone carboxylic acid, CAS number 179005-03-9) available from Mona Industries, Easley, SC, which is included with BTCA to form the desired cross-linked matrix.

EXAMPLES
The following formulations were made by: 1) adding the ingredients in the order indicated to about 50g water for each lOOg of formulation; 2) stirring until homogeneous; and 3) adding water to the final weight while stirring. SDS is sodium dodecyl benzene sulfonate.
Exanrol® A

Ingredient Activity grams/100g (wt. %)
BTCA 35.0% 18.0
NaHP02 100.0% 1.0
Malic Acid 100.0% 1.8
PCA (Monosii) 100.0% 0.0
SDS 100.0% 0.0
Water 100.0% 79.2

Example B
Ingredient Activity grams/lOOg (wt.)
BTCA 35.0% 18.0
NaHP02 100.0% 1.0
Malic Acid 100.0% 1.8
PCA (Monosil) 100.0% 0.0
SD3 100.0% 3.0
Water 100.0% 76.2
Example C
Ingredient Activity grams/lOOg (wt%)
BTCA 35.0% 18.0
NaHP02 100.0% 1.0
Malic Acid' 100.0% 1,8
PCA {Monosil) 100.0% 2.0
SDS 100.0% 3.0
Water 100.0% 74.2
The above formulations were tested for both wrinkle reduction and softness qualities. Formulation A is the control, formulation B has 3% SDS and formulation C features

3wt% SDS and 2wt% Monosil® PCA. Cotton cloths were processed as follows: 1) soaked in the respective formulations for five (5) minutes; 2) dried overnight; 3) ironed (cotton setting); A) laundered in a Kenmore® series 90 machine set to hot wash/cold rinse (12 minute regular cycle) using all® laundry; and 5) dried in a Kenmore® series 90 electric dryer on cotton (high) setting. (50 minute cycle). Wrinkle and softness data were taken after a first wash. Additional wrinkle and softness data were taken after' four more washes to investigate softness durability.
Wrinkle reduction was measured by using the American Association of Textile Chemists and Colorists' (AATCCj method # 124, Appearance of Fabrics after Repeated Home Laundering. In this method, cloths are washed and dried. The dried cloths are then evaluated for wrinkle content by comparison with wrinkle smoothness, replicas that can be purchased from AATCC. Factors such as the light used, the angle of the cloths and replicas to the light, and the background are carefully controlled and described in the method. There are six replicas with values of i, 2, 3, 3.5, 4, and 5 with 5 being perfectly smooth and 1 being very wrinkled. Three trained observers are asked to give a value

of 1-5, to the nearest 0.5 unit, to each cloth based on which replica it most closely resembles. The results are totalled and averaged over the three observers. According to the method, a difference of greater than 0.17 between the results for two products indicates there is a significant difference at the 95% confidence level. A difference of greater than or equal to 0.25 indicates a significant difference at the 99% confidence level
FIRST WASH - wrinkle results
Formulation Observer 1 Observer 2 Observer 3
A 2.67 2.67 3.0
B 2.17 2.83 2.83
C 2.67 3.17 3.17
As shown in the above data Formulation C had perceptible wrinkle reduction qualities with a confidence level exceeding 99 percent.
The cloths after the first wash were also observed for softness, wherein the observers chose those that which felt soft. Observer A chose three cloths, all washed with formulation C. Observer B chose three cloths washed with

formulation C and one cloth washed with formulation B. Observer C chose two cloths from formulation C (observer C was unable to choose a third cloth based on softness).
The cloths from the above tests were washed four more times, as described above. The following wrinkle and softness data were obtained.
After Five washes wash — wrinkle results
Formulation Observer 1 Observer 2 Observer 3 Average
A 2.5 2.67 2.67 2.61
B 2.0 2.5 2.67 2.31
C 3.0 2.83 3.0 2.94
The above data shows consistent wrinkle reducing properties in at least the 99% confidence level.
The cloths after the five washes were also observed for softness, wherein the observers were asked to choose three cloths that felt softest. Observer A chose three cloths, all washed with formulation C. Observer B chose two cloths washed with formulation C (a third was not chosen). Observer C chose three cloths from formulation C.

As such, the incorporation of silicone in the cross-linked matrix of the cellulosic fibres exhibits not only durable press properties, but durable softness properties.

We Claim:
1. A method for treating a fabric comprising, in no particular order, the steps of:
(a) contacting a hydroxy comprising fabric with at least one combination or compound selected from the group consisting of a first compound and a second compound, the first compound and a third compound, the second compound and the third compound; and the second compound; and
(b) allowing the first and the second compound to react with a hydroxy group of the fabric, or
(c) allowing the first or the second compound to react with a hydroxy group of the fabric and the third compound to react with the first or second compound, or
(d) allowing the second compound to react with a hydroxy group of the fabric, or
(e) allowing any combination of steps (b) to (d);
wherein the first compound is a polycarboxylic acid, the second composition is a reactive functionalized siloxane and the third compound is a silicone compound containing a hydroxy group, a silanol group, or another functional group that can react with the first compound or the second compound.
2. A method for treating a fabric as claimed in claim 1 further comprising the step of pressing the hydroxy comprising fabric after steps (a) and at least one of steps (b), (c), (d) and (e)..
3. A method for treating a fabric as claimed in claim 1 wherein the polycarboxylic acid is butane terra carboxylic acid, the functionalized siloxane is a carboxylic acid functionalized siloxane and the silanol is a polyhydroxy silanol.
4. A method for treating a fabric as claimed in claim 1 wherein the method further comprises the step of contacting the hydroxy comprising fabric with a fourth compound, the fourth compound comprising at least one hydroxy group.

5. A method for treating a fabric as claimed in claim 4 wherein the fourth compound is triethanol amine.
6. A method for treating a fabric as claimed in claim 1 wherein the fabric comprises cellulose comprising fibers.
7. A method for treating a fabric as claimed in claim 1 wherein the first compound is a cyclopentane tetracarboxylic acid or a polyacrylic acid.
Dated 12th day of June 2002
Dr. Sanchita Ganguli of S. Majumdar & Co. Applicant's Agent

Documents:

in-pct-2002-00766-mum-cancelled pages(12-6-2002).pdf

in-pct-2002-00766-mum-claims(granted)-(9-2-2004).doc

in-pct-2002-00766-mum-claims(granted)-(9-2-2004).pdf

in-pct-2002-00766-mum-correspondence 1(12-6-2002).pdf

in-pct-2002-00766-mum-correspondence 2(21-2-2006).pdf

in-pct-2002-00766-mum-correspondence 2(27-2-2006).pdf

in-pct-2002-00766-mum-correspondence(ipo)-(16-1-2006).pdf

in-pct-2002-00766-mum-form 19(23-6-2003).pdf

in-pct-2002-00766-mum-form 1a(12-6-2002).pdf

in-pct-2002-00766-mum-form 2(granted)-(9-2-2004).doc

in-pct-2002-00766-mum-form 2(granted)-(9-2-2004).pdf

in-pct-2002-00766-mum-form 3(12-6-2002).pdf

in-pct-2002-00766-mum-form 5(12-6-2002).pdf

in-pct-2002-00766-mum-form-pct-ipea-409(9-2-2004).pdf

in-pct-2002-00766-mum-form-pct-isa-210(9-2-2004).pdf

in-pct-2002-00766-mum-petition under rule 137(15-9-2004).pdf

in-pct-2002-00766-mum-power of attorney(21-5-2001).pdf


Patent Number 198146
Indian Patent Application Number IN/PCT/2002/00766/MUM
PG Journal Number 41/2007
Publication Date 12-Oct-2007
Grant Date 16-Jan-2006
Date of Filing 12-Jun-2002
Name of Patentee HINDUSTAN LEVER LIMITED
Applicant Address HINDUSTAN LEVER HOUSE, 165/166, BACKBAY RECLAMATION, MUMBAI 400 020, MAHARASHTRA, INDIA.
Inventors:
# Inventor's Name Inventor's Address
1 BINDER, DAVID ALAN UNILEVER R&D EDGEWATER, 45 RIVER ROAD, EDGEWATER, NEW JERSEY 07020, US.
2 MURPHY, DENNIS STEPHEN UNILEVER R&D EDGEWATER, 45 RIVER ROAD, EDGEWATER, NEW JERSEY 07020, US.
PCT International Classification Number C11D 3/20
PCT International Application Number PCT/EP00/12536
PCT International Filing date 2000-12-11
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 60/170934 1999-12-15 U.S.A.