The present invention is concerned with an ingredient preventing
viscosity problems encountered in a perfumed concentrated fabric softener
in liquid form. The invention is further related to a process for prevention of
viscosity problems in a perfumed concentrated fabric softener, a softener
produced according to the process and the use of the ingredient.
Fabric softeners in liquid form to be added in the rinse step of a laundry
cycle are well known. It is, since long, common practice that the fabric
softeners are perfumed by fragrances incorporated in the softener
composition. In general softener compositions comprise at least a
dispersion of cationic surfactants in water, see, e.g. happi, March 1995,
95 - 97. Of course, also other usual components can be present, e.g. non ionic
surfactants, anti-foaming agents, fluorescents, colourants, optical
brightening agents and the like. For example in general a common
composition of a concentrated fabric softener, which is about 3 or 4 times
higher in concentration than a normal fabric softener, contains about
14 - 20% commonly used cationic surfactant, 0,75 - 1,2% fragrance, optionally 0,5 - 1,5% commonly used nonionic surfactant, balance to 100% water.
Here and in furtherance all percent values are weight percent values
and the terms fragrance and perfume are interchangeably used within the
following text.
For example the cationic surfactant can be dihardened tallow dimethyl
ammonium chloride (available from Akzo as Arquad ® 2HT), the ionic
surfactant can be a tallow alcohol with 15 mole ethylene oxide (available as
Genapol T ® from Hoechst) and the fragrance can be any of the fragrances
usually used in this connection, e.g. any mixture of odorant materials of
natural and/or synthetic origin suitable for perfuming fabric softeners, e.g.
a floral fragance (Perfume A) or a lavender fragrance (Perfume B) or a
mixture of fragrances.
It now turned out that a viscosity problem has been encountered in
connection with concentrated fabric softeners, especially with those of the
type of the above mentioned kind. More particularly, the problem has
emerged in connection with the fragrance used to perfume the concentrated
liquid fabric softener. If a fragrance is present - and it is since long common
practice to add perfume materials to a fabric softener - the viscosity of the
concentrated liquid fabric softener becomes higher and even gelification
occurs within two months of storage time, in some cases already within
some days as outlined below. A product is gelified when its viscosity is
500mPa or higher. On the other hand experiments with the same basic
compositions but without a fragrance revealed no upgrading in viscosity.
Thus, this situation represents a serious drawback in modern concentrated
fabric softener composition distribution and handling by the end user,
respectively.
Hence, the object of the invention is to find an ingredient to be added to
the fragrance used for perfuming a concentrated fabric softener or directly to
the perfumed concentrated fabric softener in liquid form in order to avoid or
at least to reduce the instability and to stabilize the viscosity, respectively, to
such an extent that the softener can be handled without restrictions, i.e. the
concentrated fabric softener in liquid form should be stable with respect to
viscosity within a shelf life time of about two months at 37oC after the
production date. It was found that the two months stability at 37oC is
equivalent to about four months at room temperature (20-25oC).
Further, as a positive characteristic of the ingredient in case a lipase
(see below) is contacted with the active component(s) of the ingredient added
to the perfume in order to overcome the viscosity problem the active
component(s) either should not be cleaved by the lipase or if the lipase is able
to cleave the active component(s) the resultant reaction products should not
negatively influence the smell of the perfume added to the concentrated
fabric softener, i.e. the reaction products should not have a deleterious
odoriferous effect after enzymatic cleavage.
It has now surprisingly been found that when adding an ingredient to
the fragrance used for perfuming a concentrated fabric softener or directly to
a perfumed concentrated fabric softener in liquid form comprising at least
one ester of the general formula
,wherein R is a radical of a monohydric aliphatic alcohol or a group
(CH
2)
nCOOR
1 or a group CH
2-CH(OCOR
4)-CH
2(OCOR
5) and Y is R' which
is a saturated or unsaturated straight or branched C
6-C
24 alkyl group,
preferably a C
7-C
24 alkyl group, a group (CH
2)
nCOOR
1 or a group CH
2-C(OH)
(COOR
2)-CH
2(COOR
3), wherein n is 1 to 6, and R1 - R5 are each a
radical of a monohydric aliphatic alcohol, the afore mentioned instability
and viscosity problem, respectively, is prevented. Preferably R' is saturated
or unsaturated straight or branched C
12 - C
16 alkyl. Further, preferably the
ester I is a diester (Ia) or a triester (Ib, Ic) of one of the general formulae:
, wherein R, R2, R3 and R', R4, R5, respectively, are identical.
Most preferably the ester I is at least one of the group consisting of
propylene glycol dicaprylate/dicaprate, trioctyl citrate, dioctyl adipate,
triheptanoin and octyl octanoate.
Preferably the concentrated fabric softener comprises the ester I in an
amount of about 0,05 to 5%, preferably of about 0,15 to 0,5%.
If a lipase is contacted with or is part of the composition of the
concentrated fabric softener preferably the ester I is at least one of the group
consisting of propylene glycol dicaprylate/dicaprate, triheptanoin and
trioctyl citrate, because after enzymatic cleavage the reaction products of
propylene glycol dicaprylate/dicaprate and triheptanoin are non-odoriferous
and trioctyl citrate is not cleaved at all.
Propylene glycol dicaprylate/dicaprate is a mixture of the propylene
glycol diesters of caprylic and capric acids.
The other above mentioned specific esters conform to the following
formulas.
trioctyl citrate:
(tri-2-ethylhexyl citrate) dioctyl adipate:
(ethyl-2-hexyl adipate) triheptanoin:
(glycerol triheptanoate) octyl octanoate:
(2-ethylhexyl-2-ethylhexanoate)
Preferably the ingredient is added in an amount of up to 30%, most
preferably of about 16%, of the fragrance used to perfume the concentrated
fabric softener.
All afore mentioned results have been derived from tests performed at
37
oC using each time a batch of 100g of a concentrated fabric softener in
liquid form comprising:
Rewoquat WE 18, supplied by Rewo company, is di-(tallow
carboxyethyl)hydroxy ethyl methylammonium methosulfate.
The measurement of viscosity were performed using a Hacke VT 501
viscosimeter with NV spindle at a speed of 64 rounds per minute.
As described previously the effect at 37oC is double that at room-temperature.
The test temperature of 37oC is preferred because it reduces
the testing time. In all further described experiments therefore the test
temperature is 37oC.
Measurements of the viscosity of the fabric softener with the above
composition I but containing 0,9% of Perfume A and no ingredient
(composition II) compared with a fabric softener with the same composition
except that the fragrance was substituted by the same amount of water
(composition III) yield the following results.
| storage time at 37oC |
| | production date | after 1 week | after 2 weeks | after 2 months |
| composition II | 15 mPa | 200 mPa | >500mPa | solid |
| composition III | 15 mPa | 15 mPa | 15 mPa | 15 mPa |
| (1 mPa = 1cps) |
This shows that the unperfumed composition III is stable, i.e. the
viscosity does not increase whereas the perfumed composition under the
same storage conditions is instable and becomes a gel within two weeks
(>500mPa) and even a solid after two months.
Further, tests have been made under the same conditions as above with
composition II but using other fragrances. The results are presented in
Table II.
| fragrance | storage time at 37oC |
| | production date | after 1 week | after 2 weeks |
| Perfume A | 15 mPa | 200 mPa | >500 mPa |
| Perfume B | 15 mPa | 152 mPa | solid |
The results show that some key components of the perfumes may be
responsible for the viscosity increase. Therefore, to reduce the instability of
the perfumed concentrated softener some components of the perfume have to
be reduced and/or rebalanced by other odoriferous ingredients.
According to the invention the solution of the problem can be solved
simply by adding an ingredient comprising at least one compound of
formula I to the perfume used to perfume the concentrated fabric softener or
to the already perfumed concentrated fabric softener.
With the knowledge of all these results a further test series was
performed with numerous esters. This gave the best results leading to the
ingredient as claimed. The test series was performed in the same way as
above with the same concentrated fabric softener by adding 0,15% of the
ingredient. Results are presented in the following Table III.
| Performance |
| 1 very efficient | 2 efficient | 3 still reasonable efficient |
| propylene glycol dicaprylate /dicaprate | triheptanoin | isopropyl myristate |
| trioctyl citrate | octyl octonoate | isopropyl palmitate |
| dioctyl adipate |
The performance is divided roughly in three categories with respect to
the viscosity values after 2 months, viz.
| very efficient | ≤ 20 mPa, |
| efficient | 21 ≤ 40 mPa, |
| still reasonable efficient | 41 ≤ 150 mPa. |
So it turned out, as already said before, that an ingredient comprising
an ester of the general formula
,wherein R is a radical of a monohydric aliphatic alcohol or a group
(CH
2)
nCOOR
1 or a group CH
2-CH(OCOR
4)-CH
2(OCOR
5) and Y is R' which
is a saturated or unsaturated straight or branched C
6-C
24 alkyl group,
preferably a C
7-C
24 alkyl group, a group (CH
2)
nCOOR
1 or a group CH
2-C(OH)
(COOR
2)-CH
2(COOR
3) , wherein n is 1 to 6, and R1 - R5 are each a
radical of a monohydric aliphatic alcohol, overcomes the afore mentioned
problem. Prefered R' is a C
12 - C
16 alkyl.
The ingredient is also effective if it contains more than one ester,
especially more than one of those mentioned in column 1 and /or 2 of Table
III.
In addition, the interaction between these esters and a lipase was tested
because lipases may be used in a washing cycle, especially to remove greasy
stains.
The lipase works during the drying cycle, i.e. after the wet fabric from
the washing cycle, in which a lipase containing powder detergent is used,
has been handled in the following rinse step with the fabric softener. So, in
case of the use of a fabric softener containing the ingredient as described
before the lipase contained in the water remaining in the fabric, even if the
fabric has been centrifuged between the washing cycle and rinse step, may
attack the esters in the fabric softener, especially the ester of the fragrance.
The ester(s) of the general formula I with the restrictions as specified above
comprised in the ingredient preventing the viscosity problem encountered in
a perfumed concentrated fabric softener might as well be attacked by the
lipase to yield an alcohol. As said before this alcohol should not negatively
influence the smell of the fabric softener. The esters can be cut by the lipase
by the following reaction to yield an alcohol according to the general
reaction:
Therefore, the interactions of a lipase with the ester(s) of the general
formula I with the restrictions as specified have been tested with the help of
the linitest method.
A piece of fabric has been washed during 30 minutes at a temperature
of 40
oC with 2g of a commercial powder detergent containing a lipase and
was then rinsed with a fabric softener containing an ingredient to be tested
in an amount of 0,3%. The olfactive evaluation has been done as well on the
damp as an the dry fabric to evaluate the smell of the released alcohol. The
results are presented in Table IV.
| ester | released alcohol | olfactive aspect of released alcohol |
| dioctyl adipate | ethyl-2 hexanol | odoriferous |
| octyl octanoate | ethyl-2 hexanol | odoriferous |
| trioctyl citrate | none |
| propylene glycol dicaprylate/dicaprate | propylene glycol | non odoriferous |
| triheptanoin | glycerol | non odoriferous |
The reactions are as follows.
dioctyl adipate:
octyl octanoate:
The other three tested esters are not cleaved or are enzymatically
cleaved but are producing non odoriferous alcohols according to the
following reactions:
propylene glycol dicaprylate/dicaprate:
triheptanoin:
Due to the enzymatic cleavage dioctyl adipate and octyl octanoate are
each producing ethyl-2 hexanol, an odoriferous alcohol having a green
metallic smell.
Propylene glycol dicaprylate/dicaprate, trioctyl citrate and triheptanoin
do not affect the strength and the character of the fabric softener when a
lipase is present. Added to the fragrance of a concentrated fabric softener the
olfactive behavior of these esters is neutral and olfactively acceptable for an
expert panel. So, preferably R in the general formula I is a radical of a non-odoriferous
alcohol of formula ROH.
A process for prevention of viscosity problems in a perfumed
concentrated fabric softener is performed in that the ingredient as described
before is added to said softener. The addition of the ingredient may be done
during the production of the softener or after the softener has already been
produced. Addition of the ingredient to the fragrance which is used to
perfume the concentrated fabric softener is the prefered method. As the
afore described experiments signify it is advisable to incorporate the
ingredient into the complete softener soon after the production date or, what
is more recommended, immediately after the production.