Note: Descriptions are shown in the official language in which they were submitted.
9 cCo795
This inven-tion rela-tes -to liquid ~ormula-tions
capable o-f depositing a ma-terial giving a sensorialy
perceivable e~ect on-to ~abric sur~aces. The ~orm-ulation may
be used in diluted eorm and e~amples o~ the ~abric surfaces ai^e
co-tton, polyacrylic, polyamide and polyes-ter fibres, ~ool and
~lax.
The sensorialy perceivable ma-terial to be deposited
would be selec-ted to provide a desired e e eect on the sur~ace
and examples of this material are ~luorescers, ~rhitening agen~s,
I J J J
lD per~umes, pigmen-ts, dyes, bactericides, -te~tile condi-tioning
agents, for e~ample eabric so~-tening agents, an-ti-o~idants and
antistatic agen~ts.
The in~ention proposes liquid ~ormulations -~or -~abric
~trea-tment comprising
~ erO~Il about 0.5~ by wc:i.ght to about ~n~o~ by ~ei~ht O:e
~I:L':lrst disp~rscll phase consi~ti.rlg O:e particLes, beiIl~ a mixtllre
Oe
a) erom about 25% to abou-t 99% 0 e substantially ~a-ter
insoluble organic matrix ma~terial;
b) erom about ~. 5% -to about 25/~ of cationic ma-tèrial and
c) erom a~bou-t 0.5% -to abou-t 30% Oe sensorialy perceivable
material .dispersed. in
li) erom about 50~0 -to about 99.5/0 o:~ an a~lueo-lls phase.
OptlonalIy -the ~ormulation contains ~rom about 0. 5/0 -to
abou-t 30~0 O:e a second dispersed phase comprising a ~abric
condi-tioning material.
Pre-eerably the eabric condi-tioning material is a ~abric
soetener.
The -term sensorialy perceivable material is used
to de-eine a ma-terial l~hich, lihen deposited on a ~abric sur~ace
is de-tec-table directly or in~lirec-tly by a human sense. Thus a
- 2 _ /-
. .
'~- '~.', '
, . .
4~9 cc .795
perfLmle~ a prefelred material for cleposition, is an
ocliferous co~posi-tion de-tec-ted by the olfactory sense, a fabric
softener material is perceivable by -the sense of touch (-tac-tile)
and ~luorescers are perceivable by -the visual sense~ Ma-terials
capable of changing the sur~ace o:~ fabric so as -to al~ter -the
sound made during movement are also inclLuded. Some sensorialy
perceivable ma-terials act direc-tly on a hl~an sense, for exa~ple
a perfume, while some ~aterials will be percei~ecl indirectly by
their action on another subs-tance. An e~ample is a baetericide
whieh ean be deteetecd by a reduction in the odour o~ fabrics
due -to baeterieidal ae-tion on miero-organisms.
These miero-organisms will eollect on the fabrics durir~g
¦ use. Another sensorialy perceivable material providing a
reduetion in odour is an ant-l ox:i.darlt.
l6 An e:e:eeet on the sureace lr:L:ll, with some :Eormlllatioris,
he aohLeved b~ tho cleposlt:i.oll ol' the o:rganie matr:ix nl~terla:l.
That is to say the organie matrix may pro~ide a clesirable e-f~ee-t
additional -to tha-t obtained from the sensorialy pereeivable
ma-terial.
~or example, ~rith te~tiles, deposi-tion of long ehain
fa-t-ty aleohols,whieh are usable as -the organie ~at:rix ma-terial,
prov:Lde a detee-table e eeect ln respeet Oe -textile hanclling.
:[t is neeessary to ensure a mirli~ m proportion O:e
solubLe eationie mater:i.ll in ionic eorm is ln the aqueolls phase,
beeause sueh free eationie ma-terial in -the liquid phase ~rill
preferen-tially ~adsorb , or at least adsorb in compe-tition with
the par-tieles of the firs-t dispersed phase. This preference or
_ 3 - /
......... ... .... .... .
.'
': '' ,,
~ c~.795
eompetition could lead to an ille~icien-t deposition o:E the
dispersed phase on -the surface.
One eause o~ ineffieient deposition is charge reversal
of -the naturally negatively charged surface7 which can oceur if
su~eieien-t posi-tively ehargecd ions are absorbed -thereon -to be
numerieally grea-ter -than the inherent nega-tive charge of -the
surface. This reversal oeeurs with syn-the-tie polymer sureaees,
eor example -tex-tiles o e polyaerylies, polyes-ters and polyamides.
These are hydrophobie. On these l~a-terials the ne~a-tive ehar~es
are not as abundarlt as they are on hyclrc)phiLlc mn~terials, :l'or
e~c~ ple cotton~ t-3re the E)()siti~eLy char~rQd lollY are ~ler:lvetl
:CYOm oatlorlic In.llior:lcl:ls cl:lr~cl()sed heLo:lrl, the aLkyl chairl 0n
-these moleeules ean absorb onto synthetic polymer sur:eaees and
be bound by hydrophobie interaetion. Thus, -the binding o~
these eationie materials does no-t depend solely upon a eharge
in-terae-tion be-t~een -the positive een-tre oc -the eationie and
a nega-tive si-te on -the subs-trate. This ehar~e reversa:l eifee-t
was clemons-tratecl by measllYin~ ~.e-ta po-tentials by a strearning
pot~rltilL teeh~liquo on aerylie arl~l COttOII te~tiLe salllpLes. 't'hese
samples 1~ere ilumersed in soLIltiorls o:~ sodiulu ehLor:ide (5~10 l
molar) at a p~ o~ 6. On addi-tion of eetyl -trime-thyl ammonium
bromide (CTAB) a-t a s-trength of 10 ~ molar -the ze-ta poten-tial ior
the aerylie sample reversed in sign whereas -that o~ the eo~tton
sample did no-t.
The par-tiele size o~ -the ~irs-t dispersed phase ~ill usually be in
-the range ~rom abo-~l-t O.L -to abou-t 20 micron, more usually abo-ll-t
- 1.0 -to abou-t 20 micron.
-- 'I -- /- -
~ .. . . ... . . . .
~ 9 cC.79s
The ca-tionic ma-terial in the first dispersed phase
o~ tha-t phase
is pre~erably presen-t in an amoun-t o~ ~rom abou~t 2% to abou-t 10%~
The i3irs-t dispersed phase may be present in an amoun-t up to
abou-t 107'; -this range will preeerably be used lrhen the ma-trix
material also provides a sensorialy appreciable ee~ect. ~en the
formulation contains a second dispersed phase, -the iirs-t dispersed
phase will be preeerably present in an amoun-t up -to about 2%.
r~he components and parame-ters ~cor -the deposition
~ormulation T~ill no~ be considered in turn.
Or anic Matrix Ma-terials
g _ _
I-t is necessary i'or -the ma-tri~ material to have
a solubility at 25C in the liquid phase Oe no-t more ~than
200 par-ts per million, preeerably no-t more than 50 parts
per million. E~amples O:e the mcltrix Inater:ials a~re primary
or sccorlclary ~tty aLcohols O:e thc i'ormll~a ~ O~L, e.g.
stearyl alcohol, oleyl alcohol, cety:L alcohol arlcl~-tallo1r
alcohol, hydrocarbons o~ the eormula R CE3, e.g. oc-tadecane,
eicosane, docosane and -te-tracosene, aldehydes and ke-tones
oi' the ~orrnula R CO R , e.g. methyl stearyl ketone and
stearyladehyde, iatty acicls o~ the cormula R COOH, e.~.
-tallow ia-t-ty acid, coconut -eat-ty acid, oleic aci~l~ stearic
~LCid ~nd behenic ac.Lcl, and esters Oe sllch acids ~:ith -the
l'ormu:La T~ CO ORL or T~ CO OR , e.~,. e-th~l ~a:llllitate arld stcn:ryL
stearate. In -these i'orrnulae R c~d R-L are saturated or -unsa-turated
alkyl or alkylaryl groups and may be straight or branchecl chainO
~he number o~ carbon atoms ~Yill be ~rom ~ -to 22, precerably 14 to
22. R2 is hydrogen or an alkyl group l~-ith 1 to 4 carbon atoms.
., .`'
- 5 ~
. ...
,
!
~ cC.795
Other examples o~ classes o~ matrix ma-terials whic~
can be used are ia-t-ty acid amides liith the Lor~lula R CON R3R~
wherein R3 arld R4 are each hydrogen, alh~l groups ~ th 1 -to
4 carbon atoms, -CEI2CH20H7 -(CH2)30~ or -CEI(CH3~ClI20~, e.g.
tallow diethanolamide and coconut monoethanolamide. Amines with
-the eormula RN ~3R40i R RlNR3, e.g. stearyl diethanolamine and
ditallol~me-thylamine, ethers with the cormula RO Rl or RO R2,
e.g. s~tearyl ethyl ether and epoxides ~rith -the formula
~0~
R - C~2 - C~I2
e.g. stearyl epoxide. The alkylene ogide aclducts o:E ea-t-ty
alcohol~, eatty acids Ind :L'atty am:Lcles are also usab:Le as
the Inaliri.x ~natoY:iclls. 'L`ho41~ a~ ct~ haYo t~e respectLve
:L'ornlllLllo ~(a~I Il" alt20)l~0l~, IL(CLI~ ClI20)rl COOEt arld l~(CItI~5
CH20)n CON R3~4. R5 is hyclrogen or a me-thyl gro-up ancl n is
chosen -to ensure the solubili-ty limi-ts q~lo~ted above are not
exceeded, e.g. -tallow alcohol condensed ~rith an average o~
3 moles o e e-thylene o~ide, tallow amide condensed wi-th an
average oi S moles o e e-thy:Lene o~ide and olelc acicl condensed
w:Lth an average O:e 3 moles o e et1lylene o~:ide. D:i-basLc
carboxy:lio ac:icls aro a:Lso o~alllples O:e rls.lble matr:ix mclter:ia:ls.
It ~ril:L be llote-l the above :list O:r eYc.mples inc~ldes
carboxylic acids. These materia:Ls have a lolr solubili-ty in
the liquicl phase ancl ~ur-ther have a low dissocia-tion constant.
In the dispersed phase o r -the iormulation -the are abl~ -to
ac-t as a ~atrix ma-terial.
/. . .
~ cC.795
The organic ma-tri~ ma-terial ~ill be non-cationic
and Irill preferably be nonionic. The term nonionic de~ines
a material not producing ionic species in contact wi-th -the
phase
aqueous/, or pro~ucing such species only to a negligible
extent.
Cationic Materials
Sui-table materials are found in bo-th -the soluble
and insoluble classes o~ cationic materials. ~ny cationic
material used mus-t not have a solubili-ty in water greater
1~ than 5g per litre a-t 25C. Thus both cationic sur~ac-tan-ts and
cationic materials use~ul as ~abric so~-tening agents can be
used; -the la-t-ter are pre:~erred. The class of amphoteric
compounds, ~hose ionic species :is clependant on the p~l O:e the
:L:Lqulcl phas0, can also be used to provide thc QE~tionic mater:Lal
:l5 wlth selectlon o:~ the pa ill th~ system. I~'or alllphot~rlc compoun~ls, as the p~ ~oves to the acicl at a speci~ic pEI the species
becomescationic and ~ill become e~ective in the ~ormula-tion o~
the present inven-tion.
It must be appreciated -that the boun(]aries betlreen
soluble and insol~ible ~aterials cannot be clearly dra~n, thus
a c:lass oC ulaterlals generally thought o~ as solul):Le can be regar-
de(l clS insoluble ~hen the length ol the alkyl ohain or chains
are over a speci~ic limi-t. The less soluble ca-tionic ma-terials
are pre~erred because -they will no-t be so readily leached ~rom r
-the d-ispersed particles during storage; these materials ~
pre~erably have a solubility not greater than about 50 ppm.
- 7 - /
:,,, : . :
,, : :
.
:
:. ' . ~ .
. .
91L~9
cC.~95
Generic examples of soluble cationics are listed
¦ belo~Y:
j ~lkyl qua-ternary ammonium salts: R N(RlR2R3) X , e.g.
ce-tyl trime-thyl ammonium bromide ancl tallow trime-thyl
ammonium bromide.
Alkyl pyri~inium salts: R - N ~ X , e.g. lauryl
pyridinium chloride and ce-tyl pyridinium chloride.
Alkylaryl qua-ternary ammon-ium salt.s: R N(RlR2)2C6H5X-,
e.g. stearyl dlnlethyl ben~z~l amlllonium chlori(le.
LO ~mln~ ,saltg: R - N ~llR tt ~ , e.g. C12 Fr2~ N(Crt~)2~1-CII~O~,
ill wh:lch ~ arl allcy:L chalrl o~' 8 to ~2 c~lrborl atollls,
pre:eerably 12 to 18 carbon atoms,
Rl,R2,~3,R4 are me-thyl, e-thyl or propyl radicals,
X i9 an anion ~or exam~le halo~en (e.g. chloride
or bromide),sulphate, ace-tate, me-thosulphate
and e-thosulphate. -
/ . ~.
, ~ ~
.1 ~
- 8 - /
,
" : ' ' ' ~ ,
. , :
c C.79S
4~9
Examples o~ -the insol~lble cationics usable as
Eab ric softeners are:
Dialkyl quaternary ammonium sal-ts: RlR~N R3R~ X , e.g.
distearyl dimethyl ammonium chloride, dicoco-dimethyl
ammonium chloride and di(2-s-tearoylo~yethyl)climethyl am~oni~um
chloride.
Amine salt derivatives: RlR2N R3 H X , e.g. C17E35CONECH2_
NH(C~ )~C ~ )C~I3C00- and (C17H35C0~CH2C~2)2 2
Compounds with one long alkyl chain: RlN R3R4R5 X , e.g.
10 Cl7E35coocE2cH2N~(cH3)2cH3coo , wherein Rl, R2 are alkyl
chaing of 12 to 25 carbon a-toms optionally containing amide
or es-ter linkages, R3, R4 are me-thyl, e-thyl or propyl radicals,
R5 is ~, methyl, e-thyl or propyl, X~ :is arl anion, :Eor example
C L , B:r , ~ , CT13SO" , C~EI~SO,~, Cl[3COO , SO,I -
1~ E~amp:Los oC thC at~ tlotcric compoLInlls ~hictl are ~l~alJIe
are given hereltnder:
Alkyl sulphobe-taines: i) R - N(Rl)2R S03 , e.g. hexadecyl
dimethyl ammonio propane sulphona-te.
ii) R - C~I(NR13)-R2S0-3
iii) R - CII - R- S03
N~
e.g. ~
~ J
C12H33C~(c~2~3so3
_ 9 _ /---
, :. ' ,, .
:
`: :
.: :
cC.795
~mine Oxicles: RN~ O, e.g. hardenecl -tallow di~le-thyl a~ine
oxide.
CarboYybetaines: R - ~Rl)2R2C00~,e.g. C.l~H37N~CH3)2CE2-
CH2COO . Hydroxamic be-taines, ~ N+(Rl)2C~2C0~E0HCl , e.g.
C18~37N(C~3)2 ~ C0NE0~Cl
wherein R is an alky'l chain of 8-22, pre~erably 12 to 18
carbon a-toms,
Rl is methyl or e-thyl
R2 is a short alkyl chain o~ 1 to 4 carbon atoms.
Another class o~ cationic fabric sof-tening agents
usable in the ~irs-t dispersed phase is based Oll imidazoline
and has the general ~ormula
~ \ R~ ; X
wherein R and R are each subs-tantially linear aliphatic
hydrocarbon groups having ~rom 15 -to~24 carbon atoms, R is
an allyl group having ~rom 1 to 4 carbon atoms R is a
divalent al~y]ene group hav:ing ~rom 1 -to 4 carbon atoms, and
is a~ ~lion and n is an :lnteger eqlla'l to the charge on ~.
Li~uid phase
The liquid phase l~ill be aqueous 'but Irill normally contain
o~ther materials, -~'or e~ample, shor-t chain alcohols, buf~ering
- 10- /~--
: ' .
~ cC.795
agen-ts to provide the necessary pE, ~or example -to ensure
any ampho-teric sur~actan-t or conditioning agen-t is in -the
cationic ~orm, and electroly-tes may also be presen-t.
Emulsifiers, colouring materials, perfumes, bac-tericides and
surface active agen-ts are also op-tional componen-ts o~ -the
aqueous liquid phase.
An optional componen-t in the liquid phase is a
dispersed ~abric conditioning agent in an amoun~t o~ ~rom abou~t
- 0.5¦0 to about 30/0; pre-~erably this may be presen-t in an
amount o~ from abou-t 2% to abou-t 15~. This agen-t may be a
~abric so~tening agen-t; e~amples o~ -these materials have been
previously quoted in the pa:ragraph (lescrib:Lng the cat:ionic
mate:rlnls p:resent ln the l'irst tl:Lsporsccl pll~lse.
e t llo cl s c~:C p r e p a r-l t :i on
l~h:LI.e it has been :~ourl(l that severcll methocls o:C
preparatipn give the desired deposition properties certain
o~ these methods are pre~erred. The pre~erred me-thod has
-the melting -together o-f the organic ma-tri~ ma-terial, cationic
ma-terial and sensorialy percei~able ma-terial as a :~irst s-tep.
The melt may then be d-Lspersed in hot ~rater with subsequent
cooling or the melt may be soLicli~ietl ~ncl dispersed Lnto cold
~ate;r. Opt:Lon~ urther comporlerlls oI: the aclueous phase, ~Ind
the seconcl dispersed phase, may then be adclecl.
~ c C.795
E~amples of appara-tus u3able to cause dispersion o-f the
organic ma-trix ma-terial in the liquid phase are high speed
stirrers, ultrasonic dispersers, ~!ibxEIting reèds an~
con-tinuous mi~er~. T~lese ~e~ices pro-vi~le c~ erent particle
si~es ~ihich-~Yill he of ~peci-Fic u-tili-ty for differerl-t formulation~
E~amples of formula-tions of the invent-ion ~Yill no~Y
be given.
Example I
98g -tallow alcohol ethoxylated with an average of
3 moles-of ethylene oxide (~3E0), as -the organic
ma-trix ma-terial, and 2g Sudan Black B (Solven-t Black 3 -
Colour Inde~ Z6150) ~Yere mel-ted -together. Cetyl -trime-thyl
ammonium bromide (CT~B) was meltecl into -this m-ixture at the
:ro LlolY:Lng levels:
L~ 0, 0.5, L.0, 2.(), 5.0, an(l LO.Og tor each L00~ oE
mix htre o:r tEllLO~Y EIlCOhOL 3E0 and Sudan nLaclc U.
These mixtures were emulsified ~Yith lia-ter ~-t 80C
~hile s-till in -the molten s-tate, using a ~inisonic 4
homogeniser (Ultrasonics L-td, Shipley, Yorlcs) -to form 1%
concentrations.
Fabric pieces, oi co-tton -terry towel and oE bulke(l
acrylic Icnittecl fabric, were rinsed in dilutions o:L these
em~llsiorls (30g O:e emuLs:ion per lLtre of ~ater) at El l:i(luor
to cloth rat:io o-f 75:1, 25C, in a Terg-0-Tometer (US Testing
Co Inc) -for 5 minutes a-t 50 cycles per minu-te agi-tation.
-- 1~ -- / . . .
~ c C.7gs
The Eabrics ~ere remove~, and e~cess liquor -l~as removell by
a spin dryer, be:Eore -the pieces ~ere co~-ple-tely clriecl i-n a
hea-ted drying cabinc-t.
Reflec-tances o-f'-the fabrics ~ere measured spectro-
photome-trically be-fore and after -trea-tmen-t. Reflec-tances
were measured using a Zeiss Elrepho Reflec-tance Spectro-
pho-tome-ter at a ligh-t wave'length of 620 nm, and convertecl
-to K values (K = a~bsor-tivi-ty coefficien-t and S = sca-ttering
eoeffieien-t) by -the appropriate Kubelka-~lun~ rela-tionshi-p.
~he K quan-tity is propor-tional -to the ~eigh-t o:f colouring
mat-ter presen-t. ~K, -the cli~:t'erence be~tween - :Eor -the dyed
fabrie and the original fabri.c ~as computed ancl represents
~the amount of clye tahen dowrl onto l;he :I'a'b:r-ie (.ll-lring -the
r:inse.
].~ o ~l9 ~'o l l C)~9:
% ~lourl t O:r C'l'~B ~ K
. Ineorporated S S
Cot-ton Terr~ wel Acr~lic Textile
0 0.038 0.216
0.5 0.015 0.58~
l 0.053 0.~116
2 0.51~ 0.25~l
~ 0.8~9 O.'Ll~
.'~'L'l ~~
- 13 _
. .
.. '
c~ C.795
In -this sys-tem, the optimulll a~lount Of CT~B :for
the co-tton ~abric is above l,o~ arld for -the acrylic it is
be-tween 0.5 ~ncl 2C/o by l~eigh-t of -the nonion:ic. These
op-timum regions overlap be-t~een 1% and 2,oh CT~B~ where
enhanced deposition is achieved on both fabrics.
Example II
Tallow alcohol 3E0 and Sudan Blac~ B were melted
to~e-ther in the same quan-ti-ties as in Example I, and ~ere
emulsified in-to water in the manner describecl th er ein,
~Yithout CT~B. CTAB solutions were prepared and addecl
separately to -the dispersion at such levels -tha-t the r
proportions of CT~B -to the talLo~ alcohol 3E0/Sudan Blacl~ B
mixture were -the same as in E~ample I.
The mixtllres l~ore u9e~1 to t:re~t I'abr:Lcs as ln
L5 ~.xlln~pl~ ith the :eoLIo~in(r re~ults:
~ Amourlt o:e clr.~u ~lcl ecl
to the Dispersiorl ~ K a E~
~ (Propo:r-tional -to the S S
I l~eigh-t o-f Dispersed
~la-terial) _Cot-ton Terry To~iel ~cr~lic Textile
-- 0 0.010 0.120
0-5 ~ 0 '~7
' 1 0.01~ -
2 - 0.173
0.~ll56 0.:L-I'J
:L0 0.77~ -
~ 14' - /
.
.........
~,
'
~C.79~
The op-timum level of C'l'~B for co-tton was abou-t 1yo and
~'or acrylic i-t was be-tween 0. 5,h and 2C' by weigh-t o:f the ma-t~i~
material.
E~ample III
The mix-tures O:e Example I were prepared, but -they
were allowed -to cool and solidify prior -to dispersion in-to
cold ~ater. The other experimental parame-ters ~ere -those
o-E Example I.
The resul-ts were:
'10 /0 Amoun-t of CT~B K K
Incorporatetd S S
Co-t-ton Terry Towel Acrylic Textile
o 0.106 0.~89
0 5 ~).7'-'2 0 ~
'L ().~l81 l.22~l
'Ir, 2 0.~30 0.52~
0. 699 0.~82
0.710 0.211
The op-timum amolm-t O:e CTAB in this case, :L'or cot-ton,
was be-tween 0.5jo and 5~o~ and i'or acry~Lic it l~as also between
0.5% and 5% by weigh~t o~ -the matrix ma-teria:L. It w:ill 'be
noted these resu:Lts are better thcln those ql-lotetl :in Example I
~here th~ ~lisperse~l ~hclSe ~a~ d:i9~)er9ed ~iililt` IllQltel~.
The e~'~'ect ach:ieved :in Examples I, I:l and III will
be seen -to decrease in -the order III, I ancl II. This
redllction follows from the a~o~-t o-f ~ree cationic in -the
liquid phase. The method o:~ preparation u~ed in Example III
produces -the least amolm-t OI ca-tionic in the liquicl phase.
~ 15 ~ /---
, ..
cC.795
E~am-ple IV
98g tallo~ alcohol 3 E0 and 2g Sudan Black B l~ere
mel-ted -toge-ther lii-th 0, 0.~, 1.0, 2.0, 5.0, lO.Og of
distearyl dimethyl a~oniu~ chloride. Dispersions were
prepared using the me-thod of E~ample I.
The resul-ts were:
o/O Amount oE Dis-tearyl ~ K a K
Dimethyl Ammonium Chloride S S
Incorporated Cotton Terry To~el Acrylic_'re~tile
o 0.194 0.157
0.5 0.012 0.6~7
1 0.012 0.751
- 2 0.010 0.~18
1.177 0.186
L.21'1 0.~15
'L'he opt:Lrnum amollrlt o:t~ cat:ion:ic :Eor cotton :i~ above
2~o7 ~n~l:for thc acryl:ic :Lt :is l)etwe~n 0.5 arlcl 5% by ~e.i.~ht o:E
the non:ionic. '~he best le~el -for both ~abrics is bet~een 2%
and 5% ca-tionic.
E _ ~e V
Example I l~as repea-ted using dodecyl trirne-thyl ammonium
bromide (DTAB) ins-tead o~ CT~B. Tlle results l~ere as Eollows:
% ~mown-t o:~ DTAB 4 ~ ~ ~
Incorporated S S
Cotton Te:rr~ To~el A~y~l:ic Textile
_____ ___ __
0 0.21'1 0.125
0.5 0.010 0.1~2
1 0.007 0.40~
2 0.060 0.982
.4~a9 cC. 795
Example V (Contd/. . . )
~0 ~moun-t of DT.I~B ~ K
Incorporatecl S S
Cotton TerrY q'ol~el ~cr~lic Te~tile
0.229 0.803
0.329 0.464
The optimum amoun-t of ca-tion-ic for co-tton was above
2% and 1or acrylic it ~Yas be-tlYeen 0.5 and 10%. Enhanced
deposi-tion was achieved on bo-th fabr:ics between 2% ancd 10%
- ca-tionic by weight of -the nonionic.
Example ~1
9g -tallow alcohol 3E0 ancl lg cli-tertiary bu-t~l-hyclro~Yy
toluene (an antio~idant) were mel-ted l~ith 2g of dis-tearyl
dimethyl ammonium chloride, mixed thoroughly ancl allo~ecl to
sol:icliey. 'rhe waxy sol:icl ~ias l~lade :into a paste ancl then
c:rcam by ~rLrld:lr~ Lth arl :incrccls.irl~r amount o:l.! ~ater in a
pe~tle ~arlcllllortnr. Tho cre~tn l~as ~:inall.y cl:Lspet~ecl in ~iatcr,
to a -total volume of 500 ml by s-t:irr:ing for l minu-te l~i-th a
high speed s-tirrer -to form product ~. Con-trol produc-t B was
prepared by dissolving ~g O:e -the an-tioxidan-t in ace-tone
(10 ml) ancl making up to 2 litres w:i-th l~a-ter.
T~o na-turally soilecl pillol~cases were lYashecl :eor 5 mins
at ~0C in a pacldle type-washing mach:ine. AI1 unper~umecl, bu-t
otherw:Lsc conve-ntiona:l, cletergent procluct l~as elllplo~ccl at 0.2~.
Aeter rinsin~, the pillowcases l~ere C-lt in hal.E ancl one hal~
of each was ~ur-ther rinsed (5 mins at 20C) in 2 li-tres of
,
.,
.: : .
,: ,~ . . . , !
'
4~
a-ter con-tain:ing 10 ml o-f tile abvve cl:isp~rsion. Th~ other
halves ~e:re similcl-rly -t:rea-tec~ ~iith product B.
The halves of pillo~cases were then compared, :~or odour,
by a panel of 20 assessors and no s-ignifican-t di~Eerences
were io~mcl. Ho~ever, a~ter storage :for 1 ~eeh, in sepa:rate
containers, the hal-f'-treated with Procluc-t ~ l~as preferred
- -to -the control hal:L' in 35 o-~ the ~0 co~parisons. '~his
result clemonstrates -the antioxidant clepos:i-te~l in a ~ormulation
accorcling -to -the invention is more evenly deposi-ted over the
fabric -than the antioxidant in Proclllc-t B and there:rore
~upre~ses malodour~ more e~fectively.
Exam~e V[I
Emu'Ls-ions C`icmcl ~) we:re p:repared o:c' ta'L:I.ow a'lcoho'l
3~!,0 (~rl~3l?~ p~r~:rll~n~, r~ tllr(~ i..q~ lry'l (liltl~t~ly'l.clllllllon:illn
r Cil~ t':i(le (I)l.)l~) :in ~at(~:r l;o tlle :Co'LIowillg c()r~ osLt:ions:
'l'A3~ r:~ lt~ D~ C ~cltc:r~
C) 9g lg 2g 100 ml
D) 6g ~g lg 100 ~11
The methvcl o~ preparation was to blencl -the TA3E0,
per~ulrJe cmd DDAC ~y melting -them toge-ther, allowing the
mix-ture to solicl:i:~'y, then incorporating col~l water gra('lually
to ~:ive ~I coarsc d:i.spersiorl. 'rh:is ~a9 then t:re~tcd ultra-
sonica'L'L~ to :fo:rm a smo()th e~ ls:ioll.
~esin c':inished po'lyester/co-tton l'abric was rinsecl
in dilutions o r these emlllsions in a paddle action washing
-'1~- /-
~,795
machine (Ilo-tpoint Superma-tic) using a ra~tio o-~ 17 li~tres of
liquor -to 700g o~ :eabric ancl add:ing 10 ~nl o~ one o~ -the
emulsions. The fabric l~as a~Jita-ted in -the liquor at room
-tempera-ture -for 15 minu-tes, -then removecl ancl dried.
A panel of 20 assessors was aslced to smell -the clo-ths
and all could de-tec-t the difference in per-fume level be-tween
the cloths -trea-ted wi-th -the two emulsions. Those treated
with D were stronger -than -those trea-ted ~i-th C; as would be
expected from -the diEference in perf~lme con-ten-t o-f -the -two
emulsions. Both -trea-ted ~abrics were much more s-trongly
per~umecd -than one which had been rinsed in a suspension o-~
-the per-fume alone a-t -the same -to-tal concentra-tion wi-th
reference -to per-fume ag from e~nuls-ion D.
~3~;ampl c V~ J~
lro ~ dispcr~io-n l~as prepar~d, by the Inethod le~cribe(l -in
Exa~nple V[C, co~nprLsin~ ~tenryl stcarate (6~), a per~ume
mixture ((~g), (listearyl dime-thyl ammonium ch:Loricle (1~) and
water lOOg.
25 ml o-f this dispersion was then aclcled -to ~5 ml o~
a ~. 5~b dispersion o:E distearyl dimethyl ammonium chloride in
wa-ter. To a fur-ther sample of -the ~.5~ dispersion was
acldcd the sanne per:Eume m:ixture, alone, -to a level of 0.20,b.
'L'hcse tt~o d:ispcxsic)n~ wer~ -then usecl for EinaL rinse trea-tment
o~ ~ash loads.
- 1~ - /''' .
.. , ~ - ~
, ~' :
cC.795
Balanced launclry loacls contain~ing co-tton -terry -to~elling
hancl-towels ~ere ~ashed in an ~EG Lava~at Regina drum -type
washing machine ~ th an unperf-umed detergent produc-t using
-the 60C l~ash programme. Each load l~as trea-ted, in the ~:lnal
rinse, with one of -the above t~o dispersions. A~ter four
loads had been -treated with each dispersion -the hand towels
~ere assessed by an expert panel -for softness. No significant
differences ~ere :Eound bet~een the tl~O dispersions. However,
the panel were unanimous that those -to~els -trea-ted with -the
dispersion con-taining the carrier l~ere much more highly
perf~ed -than -those -treated ~i-th -the dispersion con~taining
-the per~ume mi~-ture alone.
Exam-ple IX
A clisporsion wa~ prep~lred, 'by the met'hod (le~cri'bed in
'l5 ~x~nl~)'lc 'VIL, compri~:in~ N,N-clitc~ o~ thano'lalllirlo (~
clisteaxy'l dimeth~'l amn~or~ oh'lotitle (0.5g) the optlca'L
brigh-tening agent, l-p-carbo~yme-thyl phenyl-3-~-chlorophenyl-
-pyrazoline (0.05g) and ~a-ter (100 ml).
A dilution o-f -this dispersion con-taining 50 mls in
~5 litres was used -to rinse ~ kg of non--fluorescent cotton
-terry towels ~or 10 m:inutes at room -tem-pera~tuxe. ~ similar
'load O:e towels was r:insed in a solu-tion contain:ing 50 mls o~
a 0.5C/o dispcxsion O:r disteary'l dime-thyl ~mon:illm ch'Lorlcle
~ttempts to o'bta:in a 5~0 clispers:ion of' N,~-d:itallow ethanolamine
as an addi-tional con-trol ~Yere ~successful.
_ 20 - /---
.~ .
.. . . ..
c C.795
This formula-tion is an embodiment wherein the
organic matri~ material pro~ides a desirable bene~i-t, i.e.
~abric softening. The fluorescer is nylon subs-tantive but
has been made cot-ton substantive by use o~ the invention.
E~ample X
-
16 pieces of co-t-ton terry -to~ielling (20 cms x 20 cms)
were washed together a-t 60C for 15 mins in 3 li-tres o-~' a 0.4/0
solu-tion of a conventional laundry detergent. The pieces
were rinsed -twice in cold wa-ter and separa-ted into -four se-ts
- 10 of -four pieces for -the third rinse. The se-ts of four pieces
were then rinsed fGr 5 mins in 800 ml cold wa-ter containing:
A - no-thing - thi~ ~as -the con-trol se-t.
B - 2 ml o:f' a dispersion, preparecl as in Example VII,
comprising 5% para~Cin wax ancl 0.050,h tlistearyl
'lEj cl:iluethy'l amlllon:i~ml ctl:lo:r:ide.
C - 2 Ill'L o~ a 0.0~/0 (1:ig~:t'9:io:rl ~:e (I:ig t~l:ry~ n~ttlyL
ammonium chloricle.
D - 10 ml o-f a l/0 dispersion of paraf~in wax in wa-ter
(a 5/0 dispersion was no-t suf-ficien~tly s-tnb'Le -to be
usable).
~f-ter drying, -the fabr:ics were rearrangecl into se-ts
oi` four fabrics where a set comprised one :fa'bYic f'rom each
o:~ the treclt~llerlts. These sets ~et~e then a~ses~ecl ror sot'tness
by a panel o~ 5 exper:iencecl aSSe9SOt'S. The Iorm oi~ assessment
was to ranl~ the,clo-ths in each se-t l~i-th 1 poin-t being awarded
2 1 _ /
,.. . . . .. . . ... . . . .
, . .
' ~ ~
;. . ~.
4n~ cc .795
to the sof-tes-t cloth and ~ points to the harshest. Thus,
i e one -treatment consis-tently ~ave -the sof-tes-t clo-th in
each se-t the to-tal score eOr -tha-t trea-tment would be ~0.
Similarly, i e one -treatment consistently gave the harshest
clo-th its total score would be 80.
The actual scores ~'or the above trea-tmen-ts were
A 68
B 26
~ C 55
D 51
Thus the control rinse A was no-t significan-tly
di-leerent erom ~trea-tments C ana D. Treatmen-t B gave a
signieican-tly so:e-ter set o e cloths. This resu:L-t ~as lo-und
bccausc thore wa~ not orlough so:~tcrle:r alonc to malse a
l~ s:lgnil':i.cant cl:L:e:t'cronco, but thc ~:o:Ltcncr alld p~lraf:f':ln wa~
gavo a slgnieicant ~I:il'l'crence when depositecl tog~t~l~r.
I
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