Note: Descriptions are shown in the official language in which they were submitted.
~0 ~Gl~a6~ ~9JtO3~g
2 1 990 1 ~ ~
D~ ;~r COM~O~}TIQ~
,
.
'r~c!hni~ lsld
.5 ~e ~z~e~enc i~tioJ~ ~la~e~ to ;L~uec~ uid d~t~
com~ i4~ ~ha~ comp~se a ~mc~ur~ o~ ~u~actant
n~te~al a~d to a proc~ o~ prc~a~ a~ueou~ li~L~d
d~t~ga~ co~ io~ that c~ e l~mellar ~ro~let~ o~
~u~Eac~a~t meL~erial.
lU
R~ ~kS~o~ Prio~, ~rt
L~ d~ter~ent co~q~oRi tion~ are w~ o~ che ar~ ~d
of ~ez~ ~reral ~rantages av~r sa~ id c~po~io~ or
ple, llgui~ ~o~,clc~ ar~ ea~lex ro meE~ur~, to
15 d~spe~se a~d to dissol~ o a l;~t~eri;lg llq~lor. Eu~thl~r,
llguid con~o5~t~4~9 ~i~e moro co~ o ~he co~u~or o~
being ~a~r ~nd les~ sh ~o th~ ~J~q~Pfl 4~ re~
textil~ th~c~ solid co~ ait~ ow . 'l~ -13e t~he r~a~on~
.Yhy h~a~y ~uty ar~d iight d~ty ~ullt 1~ A~ ~ i d
20 ~e~gen~ products h~Y~ ~een ga1n~n~ in p~ularlty si~
thei~ m2~ke~ i~t~oduc~lon a~ the ~xpe~s~ o~ powder~
dee~rg~n~ p~ a.
.
r~wo ger~e~al and sepa~ate clas~es o~ c~ ir,ion~
5 is~tropi~ a~ ~tsuctur~d li~ L3, ar~ the ar~
Isc~op~ c liqui~3 are lig~id~ h l ch a~ ingr~die~st~ ar~
di~olvPd and, 4antra~y tO ~truct~red l~id~, ~here 1~ rlo
struc~u~e present in i~ot~lc ll~i~l.
!
Struct~ri~g may be brough~ t to e~dow ~ 0p~rti~fi ~ch
as co.rlsu;~r pre~erre~ ~low properti~ d/or t~rbid
app~ ance. MaL~y structu~e~ ..l~i~ are al~o c~pa~l~ o~;
su~p~n~in~ paxt~cula~e solid, such as par~ic;Les o~ clay
that ~w~y be ~e~ to pro~ride a ~a~ric-~o~t~ ct to
3~ ~bric~ Les of scruc:t~red l~ d3 with~t suspez~d
~oli~s ara giYen i~ ~S-A~4,244, iB~O, whlï2t ~x ~ æ wh~rç.
AMENDED St~EEl
v~ 2 1 9 9 0 1 9 ~ 9
:
~alid p~ciclo~ axe 4u~p~ d 2~e ~clo~ed ln ~-A-~60
3~ A 3~ 10~ A~14~ 452 arld aL~o irl th~
a~'oramen~ozle~ US A~, a~ 4~,
,
5 9~2~c~r3~ }ic~ui~ can itho~ be ~tex~a~ly E~ t~red, ~n
~hich c~ss tbe ~cture i8 Co~d by prim~ ngredl~nt~,
p:~e~erably ~y surYacta~t m~L~erlal, ~ ehey can b~
ex~on:~ally ~tru~ur~d ~n w~ch ca~e ths ~ c~re ~
~ro~fided by ~ ~hree di ~ si~al matr~x ~t~ctu~s u~ln$
10 ~e~o~ary additi1~e3 liko pre~e~a~})ly ~olyme~ sll~c~e
mAterial. E~c~er~lly ~xuotu~ed llqui~ y how~fe~ pro~
~igh ~i~~ y, especially w~n 3tosa~ genoxally
ake~ t~rnally ~tructured li~ z~l o~er
excerrt~ cXuctu~
~o.~e c~ the di~fere~c ki~d-~ O~ lnter~ally ~t~;ctured
are d~Fcrlbed i~ t~e :~e~ere~e- ~tA~ Ba~3e~,
~D~te~ents", Ch.2. ~ X~ ~alter3 (~d), "~he~
r~L~stri~ 7plle~t~.0nsN, J. W~1~3y & ~ons, ~tc~wDr~h ,.9~0.
~0 ~n ge~ret.l, th~ d~gree o~ ordering ~ yst~
i~crea~ wiCh i~creaLs:lng surEacta~t andf~ el~cs~alyt~
C~C~nt:ratiO~I. At ~ low c~c~rltr~ios~ o~ ~u~ac~a~;~
arl~/or electr~lyte, ~ act~ can exl~t ~ ~ mc~lecula~
solu~iaP~, or a~ ~ solt:~tioP, o~ B~e~i~al mic~lle3, ~oth o~
25 th~ olutio~ b~i~g ~c~rap~ c, i ~ hey ar~ ~ot
~ ~ruc tu2 ed .
T~lth addit ~ ozl o~' ~4rt~ fiurra~ta~c an4/c)r ~lac~lyte,
~r~r~ous 3truature~ of ~ur~act~nt mate~lal ~ay ~orm, An
3 0 s~s~ple the2-eo~ a~e lyc~p~ uid ~ call~,ne ~ r~,
TheY~ pha~o~ may e.g. be pre~ent in ~he ~oml o~ lan~ell~r
~rwqture~ or ~n ~he ~on~ o~ ~y~al ~uct~re.
Altho~h ~en~ally ~ein8 d~lne~ aa two o~ a~ore bi-layor~
35 oS sur~c~an~ e~ o~ ~he purp~Je CJ~ ~nt;
~ell~;~ st~ucture3 ar~ ~e~i~eCl as o~ ar xore ~ aye~s o~
p~N;~Er) S~EE~ .
~lY9~19
WO 96~1U6
,
~Ea~t ant mar~r~al. Xawe~rar, pr~f~ra~ly, :L~ll~r
~cruc~ur~s a~rdin5 ro c~c in~entic~ c~tain at 1~ two
~i - layer3 oC aurtactas~ mZL~erial ~h~ce t*o ~i - lay~r~ wall
~o~m a ~ck. T~e l~m~llar ~t;:rUCtU2'1~ m~y exi~ ~n ~ar~ u~
5 ~o~ . l~ne~lar ~ ar structu:res a~ lamellar
dropl~s o~ ~ur~ac~ st bi lay~r~ ltl~e b,~-lay~rs~ ~e
~rlc~ntr~cally s~ack~d~. '
o~d tha~ ~rar~ou~ ter~ a~e u3e~ irl the ar~c ~or
~0 larne~ r 3~ u2~s. ~xas~le~ o~ ~uch t:e~9 aro a.~so~pl~
~ur~ac~n~ eha~ 15 a.g. ~e~cr~ed ln EP-~-57~,7Z3, as~
s~he~ulit~ o desc~lbed ia FtP-A-O, 151., 6a4.
I iquids wi~h la~nellar dre~1-t~ pro~ a. de~ra~1~
co~nbin~lb~ oE ~hy~lc~l 5ta~ility ~4 ~olid-~Usp~rt~na~ :
pro};e~t~ea ~h use~u~ ~low propor~o~, i.e. 1~ ~ o~ty
with ~ta~;Licy. Such li~ds ~re ~ ple l~een
de~rlbed in A. ;rurg~ , Mic~5~eruc~ure a~d Vi~ccsity Cl~
uid Det~ge~t, T~ ide 8urfacta~ t~y~t ~6 ~ 9)
~o 222 a~ ~.C~ le P~, hi~iA Dot~rgen~ e~61~e
Sur~actant~ ~Qc~rge~ a llg91~ 15~.
~h~ di~pex~ed structuring phl~e ln ll~id~ wltll la~llar
~ro~l~t~ of su:e~ac~a~ lal co~ o~ 103~1~ke
25 co~igurati~n cG~..p~l~lng c~ tric ~ y~r~ ~u~ c~t
molecul~3 ~et,we~n which wa~e~ i9 tsa~ed~ Pres~ and
ide~ y o~ bi-~ayer~ of ~ur~actant ~aterial in a l~id
may b~ nD~ aD,s ~c~; to t~.a,~ ~kill e~ 1~ the
a~t ~or ~ rle, ~ptical ~ec~ue8, va~lcu~ r~eor~lca~
~o~ ~naasurement~ ra~ ~r neutro~ dl~frac~ion ~d by ~lect~o~
mlc~cc~y. con~n~rl~ layer~ of sur:~ac~ca~ te~ial cat
be ea~ detec~d whk~ viewo~ un~e~ a t~n~ sY~o~ :
sn~cr~scol?e, ;~C~ ~s a thln ~ h~ es. Addit~onally,
~h~ b~ de~cted ~ing a mlcroscope ~ polarised .
35 ligh~ ~ mal~e~e ~ e~t~nc~lcn ~r~ pea~, th~y
c~nt~7n cos~c~ntric k~ ayer5~ ~on~"tric ~i-lay~ an
,. : .
AMENDED SHEET ! '. '
-
~ T ~ T ~ ~ . ~ . .~ r ~ --T T _ Q~ ~ T O ~.~lll--ll~l ~llW V~l~ O/~ A021
w~ ~ c~ 2 1 9 9 U 1 9 ;~ i~L~
;.
4u~th~r be detected ~ w?Ly o~ Frs~z~ ~'rac~on E~c~cr~
- M:ic~o~copy, a :~le~h~d wall~ own ~o th~ ~klll~ a~.
wo 91~0033~ di~cl~es a~u~au~ ~t~u~ur~ li~ld d~cer~e~t
5 composl~ coull?rl3i~ lamell~r dro~lcto ~f ~ur~cta~t
~r er~al . T~ co~o~ tlo~ co~ lse rela~ ly h~ gh
nc,n~on ls, e.g. 50~0Q~ by ~ei~ o~ ~h~ t~eal
~u~acca~t. The~e llquidc ~aY~ also ~een d~crl~
~h~slc~l ~t~b:LL~ty a~d ~nic~oYt2~cuxe o~ ~nGel7trate~ ;
0 ! dispersio~ r .~iauid-cr~rs~llin~ drople~o
cont;~ r~ no~ionic ~ur~cta~t~ ~n aqueou~ c~rolyte
~lution~ ch~p~rs, ~rO~ ~nd ~7an de Pa~, An~rlcan ~h~r~a
Scc~ty, ~rol. 9, 2Jo~4, ~933~ o~ th~ exemp~led
llqui~; c4~y~l~Q lamellar dxo~let~ ~o~is~i~g c: ~' a~
15 i~o~roplc co~e su~rounde~ ~y co~ce~t~icalïy J~acked
lay~r~, eb ~ p~icular ~lgur~ 4,
wo gl/09la7 d~6crtbes tha ~Y~ o~ hlgh shear ~ the
};;~e~?arae~or~ ~ a~zue~JU~ llqui~ 8oe~esge~t con~lt:lozJ
ompri.6ing~ ~ d~Floc~lt~ g pO~
~0 S~111640~ dl~tclo3e~ aqu~ou~ ul~ u~th la~ellas
~u~c~a~ ~rople~ 1 co~sing l?~ ulp~
ma~e~ial, ~a~y acid a~ ~o~onic 0ur~ata~t~.
~5
~P~A~ 3~6, 3~5 disclo~e~ a~eou~ li$~1~ dete~g~nt
c~T~o~ltio2~s com~ri~ Am~ r d~ ts3 o~ ~r;Cac~a~t
;nate~ial. a~d a d~loeculatin~ polymer h~LYlng hydzchyl~
back~ne ~d a h:ydr~ph~bic ~i~echiirl~ ~e ~y~ scla~e
scxuc~ur~ llquid~ whl~h c~r~t~;n la:mellat~ d~opl~ o~
urf~c~an~ meLt~ri~l.
.
EP~ 3ZB, ~ 7~ di~closos ~cturet li~uld dete~e~c
compo31~io~s whiC;h ~.o~y~l~eo ~0~-9~c~tJl3~d l~
35 ~rfact~ d~o~ pha~e b~ Exa~le~ XIY di~o~
liqui~l& wt ~ ~llar dtoplee~ o~ su~acta~ arlal
.
A~ENDED SHEET
,T~T~ T TC~l q~ T ~ T T -~ 0 .~H.')~13~ i Vd3: ~10.~ A0~1
219901~ ' .
(pha#e cl ~2' A so-called G-pha~e) asld a p~ue ~alle~ the
~isct~opi~ ~ece:~ge~t" which i~ ide~ti~ie~ as p~e 1~
he no.~icnlc ~u~actant ~ n ~ e XItt ~ 50~ ~y
wei~ o~ th~ total su~c~ant.
EP~ 28, ~77 di~clo~ wi ~h ~ms1 l ~r d~op~et~ a~
c~rnpri~l~g ~ n~-ou~ 3;3i3~ u~ra~tant ~late~ial wkich
i9 used as a st~bl lise~ in ~e ~ i~uid. ~lkylp~yg~uco~ld~
i9 ii~l eY ~n~ 2 Or sllch a SO~ sur~acta~c ma~e~al.
~ te~n~ te docume~ 623, ~70 disc~o~ ~id
c~n,pa3ition~ co~ri~ny ~tl~ul~r ~tabili~ors. ~e
de~c~ibed li~uid~ may compri~e hlgh ~ nic l~ ls
cont~;cioee ~al;lt~ piC dx~plets o~ sur~acta~t mate~lal
15 d-ls~r~d i~ a ~o~ uous i90troplc o~ a~iso~op~c pha~o.
~ e st;~uo~e o-~ d~o~let~ ~locculare~ and r~ o
pa~icular s~ oe~ in ar~er to be 1 r~le
;~ocu~ne~t ~' Phy~c~ o~ phiï~s M~cqll~, V~ic~e~ a~
ZC Mi~r~mul~ s" ~y ~e Gia~o ~ ~o~ 5, ~orth
;~lla:~d, di~cloae~ lc~ r l~ s w~th a la~ïlar
~L a~ ~ phase, s~e pages 17-19.
G~ 1, 06~, 554 dls~ , agueous es~l~lons ~ ln~
25 sur~zc~ant, pot~Y~i~m ~alts a~ 9'ca~ili8~ e~ial,
. .
~P A-35J, 01~ diseloa~s a~ueous li~d~ c~ ng a
ie p~se a~d ~ar~ ic ~u~ac~nt3.
~o BP-~-43~,33~ el^~s aqueou~ :Liqul~ with an aD,iso~croE;~e
~o~ ~eat) ~b4lJe wh~eh do ~ot cc2~ iso a ~ol~d ~h~se~
Ee-A-57~,723 diselc~es la~ella~ str~e~u~l c~ .yo~it~ons
eo~pr~3i~ a ~lyhy~ f;~tty ~eid ami~e a~ P-A-32~,177
~5 ~iselo~ses l~m~l 1 A~ ~t~uetu~d ~ d~ earnprl~ g
~a~llising surf ~c~a~s .
AMENDED SHEET
~ r~ ~T T.'~ T ~ _i T -Q~. ~ I n N~lH.')~ i Vd3 . NOA A~
6 j'~n3103959
~P~A-86,614 d$s~10~s a~ueou~ liquid deter~t cotn~o~i~io~
comvri~ing lamella~ droplet~ ur~act~t 3~a~esial th2l~
~y ca~ain n~o2~1c sur~acr~ 22~ oli~ -
p~:relcl~ l~e ~Ye~li~ ds ~c~at ~ ,in ~nion~c
S sux~ac~ wc~rer a~e dilu~d.
We ha~re ncw ~ a phyai~ or~ ~!o~ uld d~t~rge~t
c~po3itiot~g that ~ t O~l~y allGW~ ~re~ration o~ cally
~tabl~ uid~, b~t ~ t a'~ 94 ha~ hi~h ~or~mlati~n
~0 ~l~xibillty aAd ~a~iou9 i:~grad~t8 ~a~ i~cluded wi~hou~
advf~r~e:Ly e~c~ stab~lit~ A ~ur~e~ ad~r~t~ o~ th~ ~¦
li~id ~n iY ths h~gh e~z~ s~
~u~ r, wç h~re fau~2d ~hat l~ d ~e~rg~nt c~pa~t~o~ ~
15 .~om~ l~lla~ ~opleS~ o~ 5t~ri~act~t ~'cc;~:lal,
~er~in the ~ur~ac~ant n~erlal ~mpri~ high ;Lnrol# o~;
, ~oni~c ~ act~e, E~a~ 3h~w ~tabilicy p~b:l~, high
co~i~ies as~/or ~ drift i~ ~he ~ c~ ty u~n ~to~a~e,
isl particular at hlg~2et tem~o~atur~.
~0 :
W~ have ~ur~he~ ~u~ hlgh r~ni~;~: lit~lds cau be
r~pare~p~y~ically ~ le, lo~ cous atld/or havi~g low
~l~co~i~y ~x~l~t u~ to~ago, ~y ~nclu~ a ct;~lli~
age~t, Thu~, wo hd~ i~d tha~ ague~us ~ ete~g~t
~S co~o~it~o~ with la~nella~ draple~ co~"~,Ll~ hlg~
Oe ~ urfac~a~t zna~ca~.al c~ be ~ly ~ atQd 13y
i~cludtng a stab~lising ~o~ i~ the llc~uld. ~ e n~l~c
s~Ar~ac~a~nr CCD.t~-ring ~ id c~c51t~0n5 ~ay ~ither ha~re
an ints~aJ. ~ ial ~y~et~y ~r ~y l~X ~uch ~ ~t~ucture.
30 Th~ ~urf~c~ t in ~ne~e 1~ may ~ e ~ to 100% o~
~onios~ic ~u~acta~, i.e~ haut ~y a~ c ~ur~ac~ant
(x~io 1:0l, but ~nay ~l~o co~ n~t)ni~ and J~l~ lc
~r~ac~ he ra~lo a6 ~peci~'ie~ he~ews~or.
..
35 ~Lrthe~, w~ ha~o ~ound that ~he s~a~illty a~d/o~
de~lc~c~u~a~ lon o~ de~ge~ compositi~n co~ri~
AhlEHl)ED Stt~ET
~T ~ . r~ ' ~Tq~q~lT T~ I : ~ 1i: ()T : ~;-- [ r ~ o :~13HO\I:~W Vd3 . NO/~ A;~
WO ~C11~2~ 2 1 9 9 0 1 9
oplet~ o~ ~u~ q~ant ~aterl~l, ~4~ the
~ur f actant ~er~l ccmp~i~es hi~h levels o~ c
sur~actan~, ~ay be i~:~p~ ed ~y car6~ully adj~~ tho
~od~.um co ~ot~s~iu~ ratl~ he li~id. T~e~ onic l
~ur~ELctan~ con~F~i n~ g liq~id c~o~it~ ons ~aay e~t~r ha~re
an inte~nal ra~al ~Pet~y or choy ~ :Lae~c 3~C~ a
st:cueture. The ~u~7,e~an~ in thesq li~ds nuy eo~nprise up
to 100~ o~ no~ ie ~ aet~ . wi~ut a~y an~or.le
su~~e~ant (rae~o 1:0~ ~ut ~ay ~15~ eo~spr~s~ n~nt~ c ar~
~nl~ic ~ur~actant~ in ~h~ ~3tio a9 3~e~ d her~ex.
Fu~h~x, ~e ha~re ~oursd th;~t th~ illty a~aJor
de:~loeeul3~ion o~ uld dee~rge~t eon~o~ o~ 4c~ri~
lla~ a~oplet~ o~ sus~actan~ ~nat~rlal, w~e~in ths
1S ~u~ tan~ erlal compr~ hish le~.rols o~ nor~ ic
3ur~cta~c, sn~ be im~roved by ~130 ~clud~g ~i~h le~lg
of ~olid p~rticles in t~ 4.
Further, we have ~ou~d t~at ~he physic~Ll at~ll~y a~lor
~o de~locculati~;~, in partScular at hl~h~r t~er~uz~, o~
l~quld d3tez~ge~c con~o~ltlon campri~l~g lam~llar dro~lo~
ac~a~ ~ter~ h~ n t~a 8U~ ,Ct~ rl~l -
c~pris~ high le~ l8 0~ r~ C ~ act~t:, c~y b~
~ ro~d b~ care~ully c~o~ng the ca~diti~ o~ th~
pr~pa~atio~ p~ces~.
,
St~em~ o~ ~te~n~i o~
The ir~ve~tl~ r~r~es an a~uecus structu~e~ uid
~ rye~ cc;mp~ ion com~r~ fil l~,r ~oplets o~ ~ ~
~ur~accant m~ce~ial, ~id ~t1~7o~itio~ cc~rising a w~ht
ra~io o~ :~onloni~ ~u~cta~t t~ c ~ur~ac ~nt~ ~ha~ i~
~maller ~an g5:5 a-~d t~'c i9 hi~h~r tha~ 50:5~. 3aid
p~Yi~7 or~ catn~ri~i~g: :
i~ a ~o~io2~i~ s~ r s~b~lio~:ag ag~ c~neuirin~ a
A~ENDED SHEET
WO 96/1U62S _ P~
8 ''1990~9
suy2r u~ ool~c~ f~c~ ap~os~, ara~i~o~,
~ala~o~e, :Lyx03e, m-llnnce, gallo~, alt~o6e,
ido~e, ara~l3c~, r~oa~, tal~o, ~1~
- maltos~ c~o~e, ~ucro~ n;
ii~ a~ lea~t 1~, pr~i~rably ~t l~a~t ~ by weigh~
3f ~lid ~rticles;
iii) a~:ionic ~u_-~a~ta~t~ ~lect~d ~qm Cl~ al~l
~u:Lphate, sulpha~ate, mo~o ~a~curated ~t~y
acids ~d mix~ura~ th~eoE, w~er~ th~ ~ionlc
~0 sulphate ~ ~ulp~a~e a~ s a~ l~ast 3 c-
atGms on ~th s~dea o~ the C ~t~m ta whlch ths
Etu~p~ate or su~r~qn~t~ group 1~ att~
iv) ~n~ymes; or
Y j m ~ ~ctux~6 ~her~o~ .
The ~ ntio~ furt~r ~oYide~ a~ agweOUJ $t~c~red llgu~4
det~rgent co~po~ n cc~*rising l~ r droplets of
~u~act~nt, ~eln said su~ tant ~i~"~Llse~ e~al
20 presen~ in ~c~n~ric bi-l~ye~ ~o~n co~ ting ~ e ~r
~ore bi-~a~ o~ sur~acta~2t ~aterlal that ha~re a ~ol~o~
~ckne3R wh~ ch i# ~allsr than t~ r~dlu~ o~ ~he -~rople~,
whe~eln the cGxpo6~0n c~?ri~e~
~5 i~ a ~o~ u~a~ 9t.abili41~1g ugeD~ nt~.~n~n~ a
~u~ar ~ ec~e~ ~rom apio~
gal~c~o~ yxo~-, m~no~e, sallo~e, alt~s~,
i~l4~e, ~rabinose, ~ , t~l~g~, ~lo~o,
o3e, }actose, ~;cr~e ~ 90~1 tan7
0 ~ t le~St 10~, ~r~rably at l~t 15% by wei~ht
~ solid par~lcl~;
il~l a~l~nic ~r~acta~s ssl~c~e~ ~rGm Cl~ alkyl
su~phate, sul~hona~e, ~o~a ur~Lturate~ ~ae~
a~ds a:rld mlxtur~s t~r~o~, wher~in the a~ ic.
3 s sulyhac e o~ ~ulphonate ~o~&r~ 9 at lea~ ~ 3 ~ ~
atoms on bo~h s~le4 ~ ~- c-a~ hlch ~he
E~)E~
~_ T . ~ . r~ A~ A A ~ A~ . ~ T r. ~ ~ r r --
OT U ~ Qc~.~aac~-- ao ~ ~ , ~OT c~r~c~ T rc~ ~ Q~ ~ f~ T . c~a--T T--QZ'' ~ Tl~ !~!~LI'~,'~I~IlW V,l~ ~ AO~I
WO g~ltOG2S 2 1 9 9 o 1 9 JClJ~03~
g
,' ~ " '
3~11pha~e ~. 6ulphon~r~ gr~ 3 ~ ach~d;
~) ell2ymes; or
ixture~ r.hereof.
5 rhe ~ n~ion fu~e~ pro~ide~ a ~cc~ o~ pr~a~,g
3OUQ ~ 4~e~ge~t co~ tion~ ~ith ~a~ell~r
droE~le~s th~L~ c~m~r~ 3urfac~azQ~ ~e~rial, aid li~
c~ pri~i~g nonio~ic ~ acta~t~ at n le~tei o~ e th~n 50~s :
by wei~ht o~ 'che ~3tal 3u~ac~a~t ~atar~al, sa:~ pr~ce~3
10 co~ g t~e rn~ g o~ water, elo~roly~e ~at~2riAl a~
su~ tant mat~xial to creato a la~llar atruc~
ch~;~acteri~ed in tha~ therea~ter lamel~a~ srructux~
subjYcte~l co a ~r~shear. oper~ia~.
15 ~he Inv~lon fur~he~ 8 a pro~e~ re~2~1~y
aqu~au~ li~ia deter~e~t ca~osition~ w~h ~ lt~r
~roplets that compriYe ~ur~a~ t 2n~terlaJ, ca~
.o~ nl~ ~ur~a~tarltg a~ a 14~ol of ~nor~ th~ SO~ ~y weighc
bf r,h~ ~otal 3url~Lctan~ mater~al, who~ mixture o~
20 wa~r, ~l~c.~yt3 ma~erial and ~urf~c~ ~ate~ial
prep~re~ ~rom whi~h ~ ~liar ~t~uctux~ t8 cr~a~ed,
~:arac~rl~e~ in ~hat th~ Yi~cosity of t~ ~;Lxt~
i:~c~ea~ed ~y:
25 a~ a~ug~ g ~e Na:~ m~lar ~atio co a ra~lo o~ ~r~n 1~:1
CO 1:10;
b) by ~ n5 E;clytA~ ~:aterial;
c) ~y ~Atn~J at l~a~t S~ by weight 0~ ~oLid l~ar~icleg; a~;d
d) cotnbi~;atio~3 ~h~of.
r1~sc~ pt~on of the Irlrent~
S~ure tha~ la~ks inr~rnal r~dia~ w ~y
35 ~e li~5~ ~oxm o~ ~h3 pre~e~ Jentio~ ~ a~l96
f o~nulat ~ ~n o~ uld de~rg~nt ~osl~io~ co~pri~
AMENDED SHEET
wo~~ ]~90~9 P~
, ,,
relaci~rely high ~or~lonlc ~urfactant l~r~ i~ely
lcw anlonlc ~urZacta~t wit~o~t gi~n~ i~ on phy~ cal
5~ability, h~ g a hi~h ~o~mul~tlo~ ~lexibil~ty t~
varlous i~gr~die~c~ may in~lud~ wlthout; ad~3c~y
e~c~ing s~Lbiiity~ d ~u~ avl~ a high o~yme
s~abi} i~y ~
T~Q c~en~rl~ bi-lay~ for~ o~ the ~u~act~nt in the
dr~o~ o~ the 1~ 6 accordi~3g ~o tho i~ention con~l~t~ ~
10 o~ o~ or m~e ~ yer~ r~acran~ ~teria~ that ha~re a
j oi~ed ~c~es~ ~}sat iB smal~er tha;~ dlu~ o~ ~he
cl~opl~ . Prq~erab~y, ~he j oined ch~ ess ~ tha~
35~ the ~iu~, more pre~erably 53~ o~ ~he ~a~ , mco~
~r~xa~ly sma~er ~han 25% ~f ~he radiu3, irl ~?ar~icular:
15 ~malle~ th&n 10~; o~ the raeiu~.
.
P~era~ly, the ~;w~ ai~ accGrd~ to th~ t~o~
o~e or more conce~rric ~i~laye~ uC~Cta~é
material that ~o~ a shell whlch 13 ~e~nt o~ the ~u~8id~
2~ o ~he dro~ist. P~ferably, ~he droplet ~urt~le~c co~ri~s
sur~ac~a~ e~ial. pre~er~bly prea~nt i~ a ~ ec~n~
~o~ l~ld~ this ~hell o~ c~n~nt~ic bL~ayers o~
~u~a,ctaz-t mats~i~l. This sur4acta~t ma~c-x~zl st~y e.~, b~ ~
ent in ~he form o~ ~t~Ar ~t~tu~ec, mlc~ g,
~olutlon or li~uid ~u~ac~ant pha~. ot~er mat~r~al~, such
alt, ~/a~ and euxym~ Znay al~o he pr~ t iz~8ld~ t2~e
~ropl~t3. Px~e~ly, th~ la;nellar dro~le~s o~ r4aC~
~1~ ~ot con~ olid ~a~;icloa wi~h a ~ize la~ger ~ha~ 1~,.
Mo~ ~r~er~ly wl-~h ~ 5~,Zf~ larger than O.l}~n, mo~t
30 ~ bl~ h ~ siz~ large~ t ~2~
C~mpo~icion~ accordi~g to th:Ls a~p~ h* i~r~tion saay
contai~ ~onionic s~ acta~t~ el o~ 1~0~ by we~ght
of t:he total s~r~acta~t~. P~eE~ y, tha ~a~lc o~ ~o~on~c
35 to ~nionlc sur~ac~ s is 9~nal.1e~ tha~ 95:5 a~ ~.g. ~igher
c~ 50:50. ~o~e p~e~ex~ , eh~ o i~ ler th~
.
~.ENDEI~ ~n~tl:. :
- .
w~ 21 ~ t~
gO :13, most pra~era~ly ~ 5 ~15 . ~¢o~ pro~erably,
the ratio i~ r th~n 55:45, n~o~c pr~ra~ly highor t~a~
60;40. ~tio~ that are ln pBrt:lcul 'r ~re~rred are highe~
tha~ 65:3~, e~. xat~o9 tha~ are hl~ ~ha.n 7~:~0. Por
p~r~o~e O:e thi~ 1 nlrent~ o~ c ~o i?n'l ~nic
fiur~Ctzant ~ hC ~ io~ are ~ on th~ lonic ~o~m oe the
an~ o~ic sur~actar~,t.
P~e~ably, com}pgltion~ aceordir~ to ~~ sp~ee o~ th~ ~
10 in~ tion contain a ratlo d ~ ior~ u2~e~ , h~YiZ~y an
SO~ ~a~ ou~ re3igta~e~) o~ les~ t~ ~.4, ~o a¢~lo~la
` surfac~anta ~hat meec che ~Dnio~ie to ~ oJ~ie r~ti~. S~
d~firle~ hereu~der.
s P;~ferab~y, compo~ieioD, F~ord~g ~o t~ ;pe~ o~ ~he
illtre~ n ~urther c~,p~ X~o~ 1.5 ~o ~ ~y we~g~t o~ a
~coupl1~s p~ a3 ds~1~ed ~-reu~der. We ha~ 20un~ ~h~
li~uids with 1~ell~r ~rople~ a ~ c~ntP~ hig~ le~els o~
~o~ioni~ ~u~fac~ n ~ 3ta~ y us~g r~lati~ely
20 n~h leve1s o~ de~ polyT~er, A~Ch~a~h s~t w1dh~ to
~e ba~ d b~ an~ ch0cry, ~e~ ~olymers a~p~a~ ta s~ a
the a~ve ~ e~ iC ~'C~UctU~ . ha~ fur~he~ .
found th~t sal~d partic~6as~ n~y ~e s~pe~ded in ~ueh ll~ s
a~d the ;eormulaticn ~ y ~.~ th~C~ ~ids i~ hish.
~uldY c~nt~ r~ l~aell~ dreple~s whl~ lack a~ l~te~al
radi~l ~y~try, nlay ~ deteec~d. by way ~ ht o~
e;L~etron miero~co~y and preferably by way d~ n~asi~,
~e.g. ~ilm) or freeze ~rae~1Qnin~ P~q~ably palar$s~d
iJ ua~d ~or l~ght ~ L5~0~CC~ a~d 1~ thut ~a~ no bi-
x~rinye~c~ n in eh~ cor~ d,
depen~ ~ ng on t~ thlck~6s~ o~ th~ bilayers, bi - re~ n~e
ca~ be E~eer~`~n th~ out~id~ ~f the d~let~.
.,
We ha~r~ found tha~ by c~e~ully ad~u~t~ng ~he N~ r
r~tio, ~he a~a~illcy o~ th~ relati~ely hl~h ~C~iO~C
AMEN~EI~ SHEE~
r ~ ~ ~ o~ ~o c~ r. l ~o ~ t r c~ a ~ T ~ - T T ~ T r~ W V,~
WO ~11116:15 9 ~ Pc~rl~ui~Y
12
!14~ an be fur~her impro~ed, P~er~1y, e.~Q Na~
mola~ ~a i~ th~ llqu~ i8 at mo~t 1~ nor~ p:~e~e~ y
a~ moat 3:1, m~3~ ~re~ora:~ly at ~ t 5:1, ~ E~ar~icular
p~e~e~re~ ac l~las~ 3;~ lnC~5t; ;~ P:~e~e~abl~r, t}~e
5 Na~:~C+ molar ra~io 1~ a~ Lea~ , m5re pre~exa~ly at
ie~3~ l jB, ~.o~t pre~rably a~ lea~t 1~5. I~ p~rt~ula~
pr~ferrod i~ ~he malar ~atio o~ at lea~t 1:3. A suita~
mo~r r~Ltio i~ at l~ast
13 . .
gta~ l~g Aaer~ /t-
PreE~rablyl th~ 3ta~ilisln~ a~en~ 1~ a ~a~ionlc ~olyh~ u~
~ca~ilisiDg ag¢nt which con~ai2~ 1 ar 2 sugar u~it.s,
p~e~erahly 1 suyar ~t a~, pre~ ably, ttle M~ unt t
1~ a p~ntose or hexo6~ ring ~tructure~ ~he s~a~i$isi~g ag-~t
preFerably co~ai2~s ~se hydra~r group~,
P~e~ara~ly, ~he sugar unit is s~le~ed fro~ dl~locte~ ~uch a~
~pio~3, arabino~e, ~alactose, lyxaPe, ~n~e, galïose,
Z~ a~trose, idose, ar~ ose, rlbose, talo~"ylo~, maltc~,
l~cto~e, sucrose arld ~o~itan.
Preerab1y, ~h~ sugar ~tabilis-r co~ris~s a~ ~X~
~:id~-chai~ tha~ iB C6 or high;er, ~re~ 0 or ~Lig~r,,
25 mor~ preferabl~ C10 or hi~her; ~rom Q ~o 30 al~ylene ~e
g~oups, p~e~erably e~hylsn~ oxide groupB, may be p~os~
b~twee~ eha ~ugar ri~ a~d the alk~e~)yl ~ide ~hain; as~
th~ alXt~n)~l 9i~10 chain m~y ~e co~nected ~o the suga~ rl~y
or the ~0 g~ou~ ~y way o~ et~er or ~ter bon~g. 30
~re~err~d ~ta~llisi~ ~gencis axe 0the~fi, 6~ r~
of a~ acid ~o~ alcoho~) wi~h an alk~ yl' chaii~ a~l a ~ug~
u~ . ~ exaL~l~ of SuC~ a c~ 8 th~ ~on~ a R2~0-
NRl-Z, w~er~ln ~ a ~1~4 hydrocar~l~ 2~hydroxyet~yl,.
35 ~-hy~o~y ~yl, o~ a ~ixtu~e ~her~4, ~ CS~C~
hy~roca~byl a~d Z is a ~olyhy~o~h~oca~yl k3~1D,~ a
AM~I~DED SHEET
.
C~ Q ~ Q r c~f~q~o T r s~ c - ~ r ~ - T r - Q~ n~ V,I~ ~ N~
13 2 1 Y ~ ~.L~/~U3~'~
l.in~ar hydroc~byl cha~n, or an alkoxylatecl de~Y7,tit~
c~er~o~ es~ comp~u~d~ ~a~ .g. been de~crlbed ~n E~-A-
S7~, ,t~
5 ~ ~re~rr~ sta~ lli3'~g ag~l~t iS a ~or~i~an deri~ratlve,
m~r~ pre;~ra~lY an ~ter o~ ~o:~it~n a~e ~r~e 3r mor~ ~a~ .y
acid~ a~o;~ an et~ af oo~bi~an ~d on~ o~ moro e~
groul~s and/~r a ml~cku~ th2re4~ c ~e~ra~ly, ~he .
~o~bit ln ~ tiv~ haYa ~he ~ol~w~g ~t~u tu~e;
iO
OE~
. ' .
H~
'I I , .
H2C CX- CE~-CH~OR3
O OP.J. '.' '
~ne-rei~
- Rl 4 i~tC~2CH20) n~ 4
and wh~r~in: .
- rl i9 0 t:o 3a, px~ox~ïy to 20; and
- R'l-~ is ~ o~' C10-C20 ~a~t,y acid.
.
25 Sulta~le ccnr~o~ re polyso~ate 20 ~n ~a~, ~x ~c~;~ a
mo~lau~at0 with ES0-~0 ~ ~B~16.7~; Puly~ba~e ~1 fTw~
Zl~, ex ~CI; zL tr~ ate w.itl~ E0~4 a~13 . 3~ blcal
laura'~ ~Spa~ 20~ ex ~CI; a m~l~u:~a~e with an~ .5);
a~d Sorbltan trio~ea~e t9Qan ~5~, ~x ~CI; a trioleate with
30 ~ o~ 1.3).
Pre~era~ly, the ~n,~ohi.tion compri~e~ at lea5t 0.1%, ~x~
prefe:rably a~ l~a~ 0.5~, most pre~erably a~ l~a~e 1. 0~ by
, wol~ e,ablli~ng ~ger~c arld ~e~e~ t 20i,
35 ~n~ o~ bly ~ ~nosc lS9~ 8C ~ e~d~Ly z~ t 10~,
in p~xt~u:Lax at most 7.5~ ~y wei~ht o~ t~e e~ o~,
,,
EIJDED S~
~7.f~ ~ aq~ RR~7. RR R~ I --~7QT qOq~f~T r F~ I I r q: f ) r ~R - T r - ~7 T () N~H.'~N~nW V,~ A~2~
WC~ 0~ CI~/~g~3~,,
14 21 9~0 1 ~
.
..
e.g. a~ mo~t 5gc by wPigh~ of the c~po~t~o~,
~refera~ly, composltio~g ~ccordln~ to t~ a~ect o~ the
- ln~Ltion con~a~n a ra~io o~ ~a~ ic -~u~f~ctanc (ha~ing a~
S SOR of le~s tha~ ~,.) to dnionic ~ acrant5 ~a~ m~t th~
-s~o~iorLic to ~nion~c ~a~tio~ a~ de~ od hereu~der,
Sol:i.d Par~ ic~.es
ur~her e~b~dlment of ~he e~tio~ reLat~ to agueoua I
d deter~erLt ~o~ro~itio~s with larnel~r dro~l~t~ th~
~oznp~is~ high levels o:e nonic~ic: sur~act~t n~t:~r l ~1 a~
wel~ ~ at l~st 5~ by we~ o~ so~ p~rticl~s,
lS ~re~rera~ly, the le~rel ~ ~3ol~ part~ Cle8 '~ ac loa~t 10~ by
woigh~ r~ pre~erab~y a~ leaec 15~ by we~h~ and ~st
er~ly at l~ast 20~ ~ weigh~ P~e~ , th~ le~el
~olic;l particle~ i~ ac mo~ as~ by welghr, m~rs pro~s~a~ly
ar. m~t~ 35~ h~ wei~h~, rno~t pro~era~3ly ~ tno6t 30~ b~r I
2~ w~ig~t G~ t-h~ c~o~itio~.
Pre~era~ly, the ~oli~ p~tlc:le~ ~re 5~ rom; zealite,
s~rP, silica~ ma~ce~ial and~ r~r~ ~rq~ e
pre~e~ably zeol~te ~terlal and~o~ at~ ~;te~al,
yree~ab1y zeoli~e mate~ial.
, ' , ' .
~ ~h~u~h no~ w~ g t~ be ~und by ~y ~h~ory, it i3
b~l~e~ d that solid partlc~s noe o~ly ~*1 tc~ the
oturi~g o~ t~e li~i~ls, i3t~ als~ p~ tjY~ e
3~l, the mo~ar ratio o~ the lons 1~ the li~ o~ ec~
re~ult in ligu~.ds with l~nel~r ~roelets ~ ~ur~;~c~arl~ -
~n~tsr~al ~hat are ~no~s ~table. Mor20v r, we b~ rq that
~he ~ol~ pa~ticlss pro~lde ~ ~u~he~ ~t~:uctus~ng in ~h~
1 ~ quid which e~a~ces the p~y81cal st~1 11 ~y,
Pr~f era~ , aguo~u~ eterg~ c!~;~ it~9~9 ac~ard~g
AMEND~D SHEET
~ Cq T7 1,C~ Q ~ ( ~Q T af~q~ T r ~ T c: n T : qf~ - T r - Q7: ~ T o N~U~ V~.~: N()A A~21
wr~J~lu~zs ~ j 990 1 9 ~ J~
~o tniS ae~p~ he i~ nci~n c~e~-n r~lati~rely ~i~h,
le~ o~ nie ~Uri~5~:~CL~t mat~ri~l cen ;~0 ~o ~ta~le
by lneor~orati;l~ ~olid pa~tie~ d u~ hl~ly
eone~ra~ed 1~5~1d~. Pr~erably, ~he l~ d~ CC~ L~
5 water at ~ leYel e~ ~c ma~t ~0~, m~re p~e~ar~bly. at mo~t : -
~0~ b,~,~ weiç~he c~ ~h4 con~4itia~.
Anianic S~c .s
lq Pre~er~Lbly, c~pogiti~9 a~ca~d~ ta the i~Y~los~
comprise aA~ oni.r su~ac~es sele~ted ~ ClZ-Cl~ ~lkyl ~ .
~u~phate, C~-Cl~ al~cyl ~ r~t~, ~on4 U~CJ~U~ated ~at~
z~cldY ~ mi,x~ure~ th~e~, P~e~sraS~ly, a~oz~lc ~ur~ac~t~
are ~ ted ~rom ~Ar~da~ ~ Cl~ alkyl ~ulphata,
15 ~u:Lpho:aa~ d m~xtures ~herec~, ~o~ };re~era~ly ~ e
an~os~ic sur~a~ta~t~ molocul~ co,..~la~ ~t ~.oast 3 C-atam~
C7~5 ~oth ~1~10~7 ol~ thc C~ ~ to ~h~ t~ sulps~t~ o~
~u:l.ps~or~i7te ~rou~ is atca~ hout w~ g to 3~ ~ou~d,
beli3~0d thac the ~h~e o~ tb.e~e ~ur~ac~a~t~ a~ 9t
20 1~ ~rea~n~ th~ ~cructur~. Pro~rably, tha ra~
~onit~r~ics ~n~ these a~l~nic ~ur~7,c~s ~el~ctQ~ r~
~econ~ C12~C18 alkyl ~ te ~ ~ulpho~e a~ C~C2
-ltty aci~J i~ ~rcm 50.50 t:o 95~5. ~r~ 2rc~r~3.y,
ratio i9 ~malle;r ~an 90~0, ~7e~ ~e~
~5 as ls, Mo~c ~0~era~1y, the r~tlo ~ hl~r. ~haD. s55~S~ ~n
~ar~c~l~ar hi~her tha~ 60:40. ~Le~o~ tha~ ar~ ~r~ ~
par~icular pre~err~e ar~ hl~h~r than 65:s35, o~. ratios
~ha~ a~ra higher t~n 70: 3 0 . P~e~rably, the lelv~J. o~ e
ni~s ~ur~acta~ts i~ at le~c 5~c, mor~ p~e~ably a~
l~a~t ~o~, rnost pr~erably at 1ea3t lS~ ~y ~ igh~ he
c~pos~ior~. Pre~era~ly, ~he level c th~ 2~C~3 -
o~r~acta~ts 19 ak ~ $0%, ~o~o pre~xa~ly at mo~ S~,; -
mo~t ~r~erably a~ U~t 3~ .g~ at mo~t 30% ~y w~g~t o~ :
th~ co~Qqicion. o~n~ an~o~ic 3u~ct~ts nay also be
5 ~r~sent .
AMENDED SHEET
,
~_~ . , . A, AAAL_A~ . T _ r ~ T ~ _ ~ A . . _r~ . A r . ~ r T r~,, T A 1~ U~l~lnl~ ~l A
WO 96~10G25 16 2 1 9 9 0 1 9 ~
P~ep;~lr;~ 7tl P~O~11~9
su~prisi:~gly, we have ~ou~d tha~ a~p7 y~ pa~t ~h~x t~ th~
1 i5~uids of ~he i~rsnti~n lead~ to ~ta~ y up~ ~torage,
even upon ~t~rage ~t hi5her temperatur-~. iar t~e~ ~ur~o~e
5 of thi~ im~entlo~, "po~t-~hear" i~ de~l~ed al~o to i3c~u~;e
"e~n$ian", tenni~olo~y wsll ~ to the ~ki~led man,.
.
P~ hea~ may 5e 2~pl~d ~y wa~ xtn;~ar~ :
plel~com~cer, ~ 3h~a~ l~al~re, a col~oid ~11 or c~ ati~n~
lC the:~eo~, Shs~r rates i~xe pxef~ably a~ le~ 3, 000/~ ar~ ~ ~
pre~era~ly ~ a~ 5, aoo~ a~d pre~era}~ly ~c nlO8t ~0, 000
~o~ an ext~ la~tcrnoter, the l~acX pr~ur~
pre~er~ly ~rom 0.1 to 10 bar ~or a ~ear ~ e and th~
she~ ra~ prsf~ra;~ly ~:co~ 1,0~0~9 to 100, 300~ ~or
15 col' old mll:L .
~uxpri~ ly, ie. ~as ~een ~o~nd that the ~tabllity upon ~ -
~to~ag~ o~ ~elat~y high no~lo~ic llquld~ with ~m 1
droE~lets oan ~e im~v~d ~r creati~g a hlgh ~ coslty
~0 es~ri;ro~ms~t dur~ry th~ natio~ of lam~ d~plet~ c~ : -
s~r~a~can~ mate~ial. Without ~ hlng to b~ bou~d by any
~eorf, tt is ~ell~vo~ c~ he ll~utd ha~ a h~gh
~$scosi~y, the r~ulting li~uld-~ wlth ~amellar d~oplat~ '
will bs mo~ st~bls. It is ~th~r b~ hac ~he
~i~cosity o~ the conti~uou~ phase ~ ~he ~ wltb,
lac~a~l~r dropl~r~ o~ ~u~acca~t materlal, whi~ ~o~ Or
a :~ix~u~e of ~te~ eLe~2olyt~ ~nat~rial witho~t ~he
~urfacta~ t ~e a~ l~?o~ta~e ~ o~ ealiJ1~ ~hi5
stabili~y lmpro~ram~t.
r~lhe ~is~08ie~ oc the coIlti~uc~us ~ha~e. ;~.e. w~r a~
electrolyte zna~erial with3u~ ~urfacca~e ~L~ l, a.~d
ca~e~ue~ly the ~ Llity o;~ th~ re~ulting ll~id. w~t~ ~ ~
lam~llar draplets o~ ~urXd~ t~lal c~n b~ increased
35 :by a mochod select~d Srcm:
.'.
~ AMENDEDSHEET
~Z~:g9*~66Z ~8 fi~*+ ~*81909*01 1~+ : 9:01 36-[T-8Z îo N3H~N31-~W V,~3.NOA-A~
~oY6~1L4~ 2 ~ Y ~0 1 q
~) adj~sting the Na:X n~ol2~r ratio tO a ~atio o~ m 10 1
t'o 1:10;
b) ~ d ing polyrTIer mae~rlal;
c~ by ~ at l~a~ 5~ ~y weigh~ o~ s~ particle~ d
S ~) com~ s ~h~rec7f.
Pref sra~ y, ~h~ ~a~ nolar ra~io in th~ mix~ure o~ w~ter,
~sct~r41y~e a~ ~ura~ t i~ adiu~t~ed to a r~ o~ at '
mo~t ~: 1, more l~e~er~b~y ac mo8t 5;1~ mC~r p~e~rably ~t
1~ mo~ 3:1, e.g. at mo~t 2:1~ P~ rabl~, ~h~ ~a~:Xt~ r~t~
~t :Least 1:8, ~ore l?re~e~ably at ~eao~ 1:5 ~d mo~t
pre~ bly a~ lease 1:3. ~ a~ eio ~g ~r ~ea~t
1:2.
15 Pre~e~ably, ~olyme~ mate~ial ~9 ~dcl~d to ~h~ m~ r~ o~
water, sl~crro}yt~ and ~u~a~ant at a 10~Ye1 0~ f~n o.~ t~
by ~el~ht o~ tk~ mixtu~.
~re~ra~y, ~olid ~rticlos a~e added ~to ~he ~nix~ure ~ ~
wa~er, ~lec~roly~e ~a~erial ~ ~u~a¢ta~t ~Lte~i~ at a
l~re~ o~ at l~a~t lO~r ~y w~ght o~ ~411d ~rial, ~no2~e:
~ ly at leagt 15g~ by w3'~sht, ~ t ~o~e~a~ly at lea~
zo~ ~y w~l~ht, i~ prt~cula~ ~t l~a~t ~3~ ~y welgh~
a~ l~ast 30~ ~y we$ght. Pr~rably ~t ~no~t, SO~ ~y wei$h~ o~
th~ C~CQpCl~ait'l arl.
Pr~erably, ~h~ ~olld m~eriz~l is s~lec~d ~ro~ z~oli~,
ca~e and m~xt~r~ ~he~oo~.
~0
nr. M~
Ce~06irion~ o~ the i ~vention also co~pri3e sur~actax~e
- ma~er~at~ pre~r~:bly ~t a le~v~l 34 a~ lea~ 10~ by wei~h~
oE tho co~po~it~on, ~or~ p~rer~od ~Lt l~ast 15% by welyhc,
35 mo~t prefsrr~d at least 20~ by we~ght ~ the conpoEitl~n;
a~d pre~erably at ~ mo~t 70~ by w~igh~, mor~
AMENDED SHEET
wn 96J1062S 2 ~ 9 9 o I q ~ll~J~!~
~s
.
pre~era~ly ~t r~wo~ ~0%, ~nos~ p~e~erably at moG~ $0~ by
- w~lyht,
~rh~ surfaceaD,'c ~ erial ~y ~c~rl~e ~e o~ ~nar~ :
a-u~acta~t~ s~lect~cl ~rom ~2~ionic, c~ttonic:, ~orlon~
zwitt~rloDic a~d ~q?ho~srlc ~p~ci~, and ~nlxture!~ ther~o~.
~ ?le, they ~y be cho~ any o~ ~he cla~
cl~ea an~ spec~c ~ateria~s ~s~2ibqd i~ ISu~ce
Ac~e Agent~ ' Vol . ~, by Sc~wa~tz ~ er~ nce
~o 1~4~ a~ ~au~ac~ Acti~re Ag~T~t~' ~al.II by Schwart~, Pe~
~3e~ch (I~te~r~ e ~g5~ the ~.i4~ d~ion o~ ; J
~McCu~ch40n~s F~l~t~i~r~ te~gene~n T~uibli~hed by ~he
McC~tc~eQr dit~s3io~ ~ Manu~c~url~g Cc;~ctian~ss ~:~an,y
or ~ e~id-Ta~c~ h ', ~ . Stache , 2~ 2dD, ,, C~rl ~e~
15 ~ ~rlag, ~che~ 4 ~ie;~ sa
Suitabl~ ~o~lo;t~ ur~t~n'cs ~clude, l~ ~aztlcula
~eaccion 2roduct~ o ~otnpo~dfi ha~r~n~ a hydl~h~ e 52
a~d a xeaeri~re hydxoge~; atc~ or ~1~ hat~ c
2~ ohol~, 3ci~, ~ 9 or alk~l ~h~ w~th al~ o~t~q,
~5pl~Ciall~ ethyle~e c~5c~ ithe~ alo~e c~z with propylo~
oxide. ~p~cl~ic nor~ionic dsterge~ cor~F~un~ alkyl ~C~
Cll) p~ y o~ ~scrn~ry ~e~ o~ b~ q~Y ~;lcohols wlt~
et~yle~ oxi~e, and pr~Cu~ y c~ lo~2 c~
2s et~yle2le ~cid~ wi~h the reactlon produc~ ro~ n-
ox~d~ ~ e~:hy~Gn~-di-amine. Othe~ ~o-calle~ r~ Q~C
de~er~o2lt co~aunds ~lude lo~g cha~n ~rtlary ~1
n~i~Q~, Lo~g~chain t~r~iaxy pho~in,~ d di~yI
$ulph~des .
No2^~i.0~ Su~actant~ -
Pre~ ly, con~positio~ acc~rding ~o ~h~ Ln~r~ti~
comprise h gh 1~ 13 o~ noni~nia ~ acta~t w~ a 1
electrolyt~ ~olara~c~. It }~ n fc~d tha~ it .~S
ad~ran~ag~us to u~ ~hese ki~d o~ ~on~ u~act~nts ~o
AMENDED SHEET : :
T ~ ~ T T r~ . . T_~7 . ~ T . r~ T T _ r~~ . T ~ I~ I--r~ rnr~l U_l _r ' I~ n A
W~ U6:~j 21~'~ ol 9 pc~r~Jr~
1 9
~a~ cture oE c~e l i~ s ~E the p2~e~t
e~tio2~.
Compc~ ician ~ ~he lnvention pr~era~y c~lnpri~ no~ios~lc
S ~ ct~r~ h~Ying a:~ ~OR o~ leR~ 6.4, ~rsfesa~ly le~
tn~ 6.~ herein pr9~c~ d ~or electroly~e
~lexa~c~ e:~aed ~he mea~ure~nt of ~ul'clng~out
~5 ~s~anc~ ~S02~. ~or thi~ t~gt, 200 ~ LS pre~r~d o~ a 5%
~y w~ight 3~IU~o~s ~plutio~ ~f e~ ~3U~;3C~U~t ~n ~eee ~ cn .
10 ~riso~ n~ra~o~ri~cetate ~A) 1~ added ~t ~oom
t~ps~a~u~e ~c~ a5~c~ untiï ~ha3e ~epa~aticn ~ccur~, as
c:tbE~e;~r~:d rh0 o~et o~ clou~ h~ o~ NTA adde~
at thl~ pc7~t, ~5 oxprR~0ed ~;c~ gra~ e~alent~ ~dtsd t,4 1
lit~e 3~ ~he ~u~ac~t~ ~olutio~ r ~TA ~ 3 Yq~
1$ the ~altin~^ ou~ re~ ce o ~h~ tactant . Where
con~eni~, th~ abb~ ie~ Sc~ w~ll b~ u~ x ~tl~g-
out ~esiY~a~ce~ : :
'
Pre~era~ly, the weight :ratlc o~ nl~c ~ur~actant w~ a
~C SOR of le~ t~ 6.4 ~ icn~c ~ur~c~ants iY 3malle~ than95:; ~nd high~ t~n 50:SO. Pre~era}3ly, ~e ~t~o is
~L1~ t~ 0:10, mo~e preferably ~alle~` ~,han 25:15. 1
Pre~er~3ly, th~ r2'cio is highe~ t~a~ 55:~S, ~ ~e~ably
~ighe~ t~ ~0:~0, most pre~erably higher th~ 65:35, q.~. -
25 hlghe~ 'ch~ 70:30.
.
~ddi~lo~ally, cc).~c~ r~8 0~ the ~re~t in~ nay
pr~ ra~ly ~rthar ¢~rprl~- ~urfactant meLterial ~Ac~ud i ~
nh~ reic ~uxfacta~ lal~ wi~h an ~0~ o 6.4 or hi~her. .
3C ~lthough nc: t wt~ rJ ~o }~ y as~y t~f -- y, lC ~5
~e:liev~d that a higher l~Yel G~ ~urfacta~t" Wi~h hlgh~r S~R:
n)a~ l~a~ to ~uids wlth dropl~ts t~t ~how inc~ r dial
8~e~
35 Arllani~ S~r~ ,~t~s
C~mpr~ition~: o~! th~ se~ ~nve~ior may ccD,~ain sylltheel~
. : . .
... AM~NDED SHEET
ca~ ~Q ~ hQ rc~nq~T T~ ~q ~ nT q~- T T -Q7~ ~ Tn ~^~ ~nw v~ \IOA
W~ 96/1~6~ 2 ~ 9 ~ o ¦ 9 i~--'TJ~;pr~"'3~
ur~io~ c su~facca~t 1A~ nt~ ~hlch ~r~ pre~era~ly
pr~so~c in co~l.~tl4n wi~h ~he ~bo~e m~tio~e~ ~oD~lon~c
r~Lterials- Sulca~le a~ioni~ ~ur~c~ t~ a~e ugually ~t~X-
solu~1~ alkali m~l~al ~alt8 of organlc ~ulpha~ea a~
5 sulphonat~ hav~g alk~yl r~C~1~ ¢C~ r~m ~clst 8
! tO ab~ carbon ~t~, ~he te~ alkyl bel~g u~ed to
~rlclude ~he al~ll por~io~ o~ hi~h~:~ acyl r~ L~ 8
o~ ~icable sy~ ic a~io~ic sur~actant ccmz~ ar~
sodi~.~m and ~orassium alkyl ~lphate~, e~ci~lly tho~
~0 obt~ln~ ~ sul~haci~g ~lghe~ ~C~-C~ lcchol~ p~oduc~d,
~or ex~npLe, ~om ~All~w or COC4~Ut oiI, 9a5~um ~nd
~otêaa~ium allcyl ~ Q~ be~zene sulphQn~5~ p~rt~ ly
a~di~ lin~ar seccn~ary alkyl ~C~O~C~ en2e~e ~Ul~hn~t~;
~orl~ m a:lkyi glyce~ol ~er ~ul~hates, ~eclally tho~e
15 ~3~he~Y of t;ns high~r al~oh21~ de~iYed ~r~n callow or
cc~o~u~ oil ~ the~ ohals der~Ye4 ~rom petro~
~odi~ l::OCO:~Ut oll ~d~ty mon4~1yc~r~d~ sulp~e~
~ulphonace~; w~i~ a~d po~a~siu~ ~alt~ ulphu~ic ac~d
esters c~ highe~ ~C~-C,,) ~atcy ~ oh~l-a~ e ox~d~,
20 pa~iculaxly ethyl~e o~ re~c~ p~cduct~ e
~actlo~ pr~luc~ o~ atey ac~ds suc~ a~ cocosu~ ~a~t~
~ci~ ~s~e;ri~i~d with i~ot~onic acid ~d ~eu;~ral~zq~l w~-th
~odil~m hydrox~de; scdium a~d ~o~a~ lt~ of ~a~'cy acl~
an~de~ o~ yl caurl~e; al~ear~ Tt~v~t~onate~ ~uC~ a~
25 tho~ de~lY~d ~y reac~g ~ le~ s ~C~qj w~th ~
bi~uLphi~e ~ those ~ri~,re~ reacti~g pa~ w~th
SO2 ~c~ C~ and thon hydrol~sing with ~ ~ase to ~xoduc~ a
ra~d~ su~pho~ate; ~n4 ol~ ul~oDateq, w~c~ te~ i3
~ed ~c desc~i~o tho ma~erial ~at~ by reac~ cle~
30 F~ u~ar;y Clo~C20 al~alo~ins, with SO~ and t~
s2eu~ra~izi~ a~ hydrolysing the ~oa~tio~ pro~uct. Th~
~re~e~red ~n; onic 51~2aCta~l~ CC~tpOU~ldS a~e sodium ~C~C~
~lkyl b~nz~e ~ulphon~tes a~d ~o~ C~- Cl~i ~llsyl
~ul~h~es .
It is al~ po~ible, a~a some~ime~ ~r~er~eqi tO i~cl~de ~ ~ .
.
AMENDED SHEET
: :
AC~I~ . OOI.~'O-- L~O ~11 ~lOTOA~. AT T~ 00 AT O
WU~t~/lU~Z5 2 1 ~ 9~J 1 ~ r~ rJ~ ~Y
21
alkali ~netal soap o~ ~ mono- or di-car~oxylic: aci~,
~ ~c~ally a ~ f a~ acid ha~ g Xrom 12 ~c) 18 carbo~l
a~r~; Xo~ ex~ o ol~i~ acid, ric~olelc acid, alk l~ yl
t~ e~ dodecyl 5UC~ , a~ ~atty aci~l~
5' ~e2-1Yed fro~ ~astor ~ ap~ceed o ~ ', g~ound~ut c~l,
ccconu~ o~ k~Lel oll or mlx~ures ther~ d~
~r p~ iu~ aoa~ o~ the~e a~ids c~ b~ uc~
n~h~r ~sur~cr;~nt r~terial.
10 ~ hl~ ig ~he u3e o~ 5alti2lg t~ eigtar~t active
ial~ such ~6 :Eor ~ 10 d~c~ibz~ in ~P-A~,328,1~7,
esp~cially the u3e ~f allsyl~olygly~5ide ~ur~ct~z~ts ~uch
as ~or ax~;~pie diYclG~ed i~ ~P-A-7~, 074 . Al~o ;~lk~rl ~ono
g~uco~id~s may be used. Pu~ther, ~ yl gluco~e ether may be
15 u~ed ~L~/c~r ;~olyhydrox~ ~ae~y a~id ~ a~ d~scrlbed i~
~00 ~0~1~7, ~nor~ pD~rticular the ~ use~
Exampl9s th~reo~.
lPctrolyt~
20, Com~c5it~ s a~o~di~g to the inv~ntion m~y ~pt~on&~ly al~o
cantai~ ct2~1y~e ~n a~ amou~t su~ le~t ~ b~l~g a~ou~
s.~ucturing cE the deterge~t actl~re ~ rlal. ~e~ra~ly,
t~a ct~ ia~ con~ ro~ 0~ ~referably 7~ o 60~,
~p~c$ally ~rom 5~ x,~ly 10~) t~ ~L5~ ~ a Ja~ g-ou~
25 eïectrolyte. S~ y ou~ trolyte ~as th~ nlr~s
a~cribed i~ ~pec~icatlon ~!P-A-79, ~46, that i~ al~
~lactral.yc~s ha~ lyotro~ic n~er o~ l~s~ t~ ~.5,
preferably le~s ~ha~ 3 . O . Prefex2~ed ~alti~g~o~t
eïectro~yteY are ~ole~c~ed ~r~ alkali meta~ a~ ~o~ium
30 ~lt~ o~ ~h~pha~ clutln~ py~o, ortho and poly
pho~phats~), silicates, b~r-6~ta~, c~on~e~, 3~1p~t~,
~itrat~ ~itriloacecat3 a~d ~ucci~uLce~.
. .
Ruilder~. '
35 ;~ is pre~rred that c~np~ ~ ti~ns according to t~ pxo~a~t
i~ i.nclude dete2ge~y b~ ns~ri~l, 30sn~ or ~ll
AMENDED SHEEl
TC~I ~ C?~ C'-- ~0 ~1.1 l~T~n~ T rc~ r . ô~_ r T _O~ . T;~
2 i ~ Y O 1 9 ~ '~35'
a2
!
of w~cn m~y ~e el~c~r~lyte.
Exa~les o~ ~hoc~horo~ cn~ta~ ng in~r~anlc ~er~e~cy
build~r ir~clude ~he wat~r- soIul~ alt~, esp~cially ~
5 ~ecalpy~op~;os~ztes, orthoph~phate~ ypho~)~tes and
~ho~h~na~e~. g~eci~.c exa~pl~B o~ lno~ga~ic ~lo~p~ate
builde~ ir.clu~e sodl~lm and potas~{~m ~ripoly3;~osphate~,
~h~sph2te3 ~d hes~rn~ h~?hate~ Pho~ph4n~e ~ R~ra:clt
buil~ero m~y ~ïno be wot. SQt~ lc i~ h~
lC p~e~e~ n~ e th~ aur~nt o~ ph~h~ ~lldo20.
~a~r~ e~ o~ or~ phcsphcnl~ ~cont~ i n Ln~ inor~ c ~a~e~e~
buil~esrs, whe~ presle~ D.clud~ wate~-801~ble al~;Llt ~net71
car;bonat~s, ~ r:~on~e~ L~ca~e~ ~d c~y~tallln~
1~ ~hous ~ ilicates, Specl~lc ~plea i~clu~
sodiu~ ~r~o~ (with o~ w~thaut calci~e g20dJ~ tas~
carbcn~Lte, 60dium a~ put~ ~n b~c~r~tes, silicates an~
1 ite~ .
20 ~Ampl135i~ 0~ orgaz~ic ~leterge~ ld~rs, whe~ ~eflo~:t,
ln,clu~ the alkali~e met d ~ub~t~t~d
2Ut~tl4~1iUm pclyac~tate~ o~at,cs, ~O~yc~r~Qxylates,
p~lyacetyl carbo~ylate~ a~ ~lyhyd~ rs~lFh~te~
8~f~Ci~iC sx~es i~c~ iLun, potas~a~um, li~h~
~5 ~ a~d substitu~ alt~ ~f ethyl~e~ nP-
tet~aacetlc a~cid, n:i~rl~ ot,J:l~cetic ac~d, oxy~i~uceiD~e
ac~d, melitlc acid, b~ ene polyc~oxs~lic acid~, Cl!~8,
~rSrate ;~o~;o a~lCCin~te, tar'crat~ di ~cCi~ate and ai~rlc
. Ci~ric zcids or salts th~rQc~ ara p~e~e~red bu~lder
30 ~n~Lcorials for u~ç~ in com~c~itio~ o~ ~he inve~:t1~n.
In tho co~text o~ or~anlc ~ilders, it is al~ sl~Le to
l~cor~ora~o po~ner~ wh;lch are only ~a~tly ~ls~o:ltrecl, in
~he aquecu~ cc7~ 0us phaso a~ deec~bed ~r~ EP~L 3Cl,88~.
~5 '~h~ ~ allo~s ~ c08i~y ~educ~io~ ~due ~ ~h~ polymer whi~h
1~ d~ss~ d~ whil3t incox~oxa~l~s ~ ciently hlgh
~ E~E~S~E~t
a~RRQ;~ ~Q R* l : ~Q T q~-q-b~ l T ~ qq - O T qR--T T--Q~ ' T O \I~I~ ll lW V~1~: !~10A A ~
W~ 2 1 '~ 9 0 1 ~ ~ ~ P~ u~
.
~nou~t to &chie~ ec4~da~y be~e~t, 3~ecially ~ulldi~g,.
~ec~ the part ~h~ch i6 n~ dl~sol~ doe~ not b~i~g
abou~ the ~t;~ility t~a~ would o~cur if sub~t*n~ ly ~1
we~al dis601v~d. Typioal am~unt~ are fron~ 0.5 ~o 4.5~ by
S w~ight.
ere:~era~ly the le~el o~ non-soap bullder ~zLt~rl~ c~
5~0 ~ w~ight ~f tk~ ~nposlt~on, m~re pret'~ d ~om 5
t~. ~5 ~ b~ welgh~ o ~he ~:o~po9itio~.
~O
Decou~l :inq Po~rler
Pre~e~ably, composltio~ ~cco~ o the p~ese~t~ ln~r4~tio~ ~ ~
t~2e~ comp:~i9629 ~rom 1.5 to 5~ ~y wei~h~ o~ a A-c~
~oi}~ r ~el~te4 ~x~m de~occula~g ~ol~mor :ha~ a
1~ hyd~ophilic back~ d ~e ox mq~e ~yt~o~ho.bic side~:
c:h~iz~, o~ bein3 a ~lock c~oly~r havi~g al~ers~ati2~
}.ydrophobic and hydro~hill~ groups, or haYlng 210~ ~C
a~d io~ic ~llel~B.
'
20 S~ al types o~ ~e~ cu~d~g paly~re;~s ~a~e ~e~
d~c~ d ln ~he ar~ . EP~A-3~L6, gg5 ~8crl~ e~loccul~t~
po~ rs ha~i~ a l~y~l~ep~ c back~on~ a~d o~ or
hy~rophobic 8~,d~ ~h~1~q, t~0 91~06622 de8c~$~e~
~Xlocculzt~g poly~ra ~el~g a ~lock copolym~ c~ t~g
~S ~ alt~ ng hydroph~c ~ hy:lr~ ilic ~;~uU~, W0
~l/O~Z3 de~crlbe~ de~locculatlr~g ~alym~r~ COXI ti~
~a~icrLic r~onom~rs and io~lc mo~o~nar~ ar~d G~ 2 237 ~13
describe~ de~loccu~atir~g ~lym~rs co~letln~ o~ ~
hyd~opkcbic h~hor~ a~d one or laoro hydr~ c ~ide-
30 c~ s.
,
Prefer~bly, the de~loccul4ting p~:ly~e~ er~s~t a~ alè~ o~ ~rom 1.5 to 5 '; ~y weighc oi~ ~h~ ~o~t~on.
3`5
P~ bly, sompo~i~ion~ c~ ~he ~0~2at i~re~tlon a~
, .
AMENDED SHEET
. . .
~ lLo~; 2 ~ ~' 90 ~ 9 ~` f~;~5'1~
2d~ .
cc~cenCr~C~d. ~rhore~re~ the w7.t~r le~ol in ~he 11quid,
~e~e~ comp~s~tio~ ~cor~g to t~! E;r~e t ~ tlc~
i~ ~re~e~abiY ~t l~st 10~, mo~ p:~efe~a~ly a~ l~a~c 20~,
mos~ pr~er~bly a~ l~aat 30~ by welgb,~ ~ th~ c~si~o~
and pr~erably at m~8t 60~ by woig~3t, nlo~ pr~ exa~ly a~ :
mo~t 50%, mo~t pre~ra~ly at ~no~t 40~ eigh~ of the
~n~osition.
O~o~lal Ina~0d.i.~
A~t ~ sn th~ i~g~ed~e~co al~aty m~t~one~, a ~er f ~¦
. opt~onal lnyre~iqnts may al~c be ~e~ r ~a~e
lat~q~ booscers such a~ no~ , p~c~a~ly the
mo~tha~olamld~s d,~ri~ p~lm k~z~el faety aclds a~d
coc4nu~ faety acid~, la~h~s d~rQ~nt~, oxygen~ relea~ng
ble~ni~g ~ such ~ m p~ r:~ts a~d ~odi~n
perca~a~a~e, p~raci~ hleac~ ~rocu~3cr~, ~hlor~,e-releaal~g
l~le ~hi~ a~ uch a~ trichlo~l~ocya~uric acld,
i~o~ga~ic salts ~uch a~ sodili;r. sul~te, a~d, usua~ly
~0 pres~A~ re~ r~ o~ amou3t:s, ~luo~c~t a~t~,
per~umes, enzy~es la~c a l~,rel of 3.5 5~ ~ wei~ht) ~u~h 3S
protea3e~, ~la ~ pas~ (in~ludin~ ~lpoLa~3e ~
Ma~k) ex Nc~c), enz~t~ 3tal:~ilixe~5, an,t~ pn~lit~Cn
ag~n~s, g~z~ R and colo~ts, O~'OU3~y ~2~ sel~c~
~S the mat~r-l~Ls ~tn~ ~han ~e pol~r for u~e in
co~poYi~ion~ o~ e~e~on, a~o bi~degradab~e ~at~r~a~
~r~ preeo~ed ~ox en~ l reasa~s~
;.
Pr~uc~ Pr~rtie~ ~
Co~np~sicicn~ o~ th~ .v~nt~o~ pre~rably ~a~c ~ co~y
~f Les~ ~n ~, ~0~ mPas at 21 9~ or~ pr~err~d 1~5 Ch~
1,5~0 mPa~, moo~ ~efer~4 le~ thc~ 1,300 ~a~ gher
th ~ 10~mPa~, especially pref~rre~ ~etwe6~ lC0 ~ 75û mPa~
~ 21
c~ icions a~co~di~g t~ ~he in~tlt~n ~e
Al\~ENDED SHEEl
~7~.~:q.'~7r7RR~7: Rl~ Rbl ( ~7~T~()~70r Tf~+ : ~5~ R-rr-R~ i N~lH~N~ d~-NO/~ .'\~:)~1
W~ ~f1062~ 1 ~J 9 0 1 j ~C'L~/~.WW~SY
phy~ic~Llly ~ a~o a ~lativ~ly lo~r lfiscoslty, ~n
- ~he corltext o~ the E~es~nt ln~ren~lo5~, phy~ ility 1~
d~ La~ o~ th~ ~A~ m separatia~ co~pa~le wi,th -
~1109t ~r~a~ur~g ~ reta~ r~n~cq ~le
5 co~n~s~ ~lon~ will ylel~ n~ more th~ 10~, p~ ra~ o I
~n4re than 5~, ~gc p~eEerred zlO mor~ tha~ ~% by v~
pha~e seya~ation a~ s~i~Pr~ y a~ea~ o~ 2 o~ re
~e~ara~e pha~e~ when ~cred Eit 25~C ~or ~1 d~y~ ~r~m th~
t~me cE pr~parat~
~0
P~erably, li~id c~ros~ o~ 0~ Ch~ ~n~r~n~on ~ ve a ~i
o~ between 6 ~r~d 14, more p~e~err~d ~rom ~ tc 13,
especially pre~erred 2~m. 7 ro 12
15 Pre~ex~ly the pH, as pro~r~ ded tc the wash ll~ucr, ls a~
l~a~t 6, moxe ~re~ ly ~t; lea~t 7,5, ll~0l3k ~r~e~ly at
least ~. Pre~ra~l~ t~e p~ i8 at mo~ ~2, ~r~ pr~erably
a~ o~ r3~1y ~t mo~e ~,
2 0 ~etho~l o~ P~p~rat i~
Ap~rt ~ro~n th~ a~ove ~e~t l one~ ~ro~ pr~p~ti~n, a
p;:e~e~ed ~ethod ~or ~he ~r~pa~at~ on of ~quid det~ge~
co~r~os~ons in~al~es ~ch~ pessing o~ the elec~rolyt~ ~ ~
i;~edient (i~ ~re~euc~ ~agether ~i~h t~e minbr i~gr~t~ t~
25 exce~ or ~he ~ rature s~ ive ingred~ a~y~
~r~ wa~ o~ el~od te~ ratu~ oll~w~d ~r thel add~tion
o~ ~h~ er ~t~al~ , the d~t~5er~t acti~e
m~toeri~l ~p~lbly ao a pre~$x~ rlrls a~d
th~a~ ~r cooli~g ~he m~xtLIra and ~ any te~npe~ature
30 8en9i~i~re tni~or ingFe~l~c~ ~u~h ~8 /s~a ~ tc.
Th~ d~ c~lati~g polyme~ or ~le ~e added a~er
th~l ~le~roly~e ingr~dle~c or as the ~ ingredie~
Pre~erabl~l, the de~ ol~Z~ are elCl~d pri~r to
the Eo~ on o~ ~he le~ll~ ~ctu2~.
~L~ use ~ d~ter~e~t cam~it~ons a~ ~he ~ lcn wlll ;~ ~
p~ENDE~ SHEE~
U,~ 5' ~0 ~ ~QTaf~a~r r~l : Rq:nT : ~R~ RZ:: 10 N3H:~N:~l.lW Vd~:NO.~
W~YbllUOi~l 2199019 ~r~^
26
dil~ed wi~h t~ r~h w~r ~o for~n a wash llquà~ ~or i~sta~ce
~c~r u~ ln a washlng ~aehi~e. T~ ~o~centrat~o~ o~ l~quld
~erg~nt com~?o~itio~ i~ the ~h ll~r ~g ~r~era~ly ~ron~
0.1 ~o 10 ~ 3~r~ p~:e~red ~om 0.1 to 3~ ~ w~ght.
~:he in~v~ti~ will ~ow ba ~ st~at~ y waLy o4 the
~ollowiny ~n~ lixlting ~x~les .
p~ E~E~) S~
A,A , . A _ A~_A A ~ ~ r~ T ~A~ T T A ~ . A T . ~A _ T T _ 05' . r A ~ ~LI ^~ lnlA;
wt:~rwlu6~ 2 1 9 90 j 9 .. ~ .P~t~
.
EX~MPhB~'
~x~
Th-3 f~llowing co~..yo3$tions were pre~ared ~ s~ g ~he
S lng~dien~ h0 ord.~r 1 i~tad
FORMl~ TI~ ( i n wt ~
Watqr 16 . ~3 1~ 3
~CO~ Sol (~s~ .27 13 . ~7
Citric acid ~a~hydrous)7 . ~ 7, o
Glycerol ~ ~17 ~ . ~7
Borax a . g2 ~ . g2
Ze~lit~ 1~ . O
P~ 8~ . . S 1 . 5
l:~S ~cid* 6.25 5.~5.
r:ob~nol 23 ~3~OE~ 2) 13.33 13.33
~c~ 3 E6.~ 3) 13.33 13.33
~5~ 0* ~ ~.0
M~ n~rs 1. 8 1. 8
Ph~se sep~rat~ (d~r 2
moJlths ~ 45~C: i~ ~n) 0 5
Na ~ ~ X I ratio 1~
.
~S ~ Th~e ir~:Ce~ eD.C~ we~e added as . a ~remlx
1) Pslym~ Al' oi~ EP 346. 995
Cl~ t~ C13 ~ni~niç ethoxylated with on ~ ~63 3 EO
~ou~ x Shell .~
3) C12 ~o C13 nonionic et~4~ 0~ wlt~ on ~e2~ago ~.s ~O
30 groups, ~x Skeil
~ Sor~ta~ lauraee, ex ICI
Th~ com~o~ition w~h tl~ s~abll~s~ ~hawed no phase
~ eparatic~ wi~er~PS the composi~ior~ wit~cur haCl a 5
35 ~eQa~Ltion up~ r~g~.
:
....... ~ ..... AhtE~lED S~t~T
~ .:
~#: S'9bb668c. 68 6~+ ~81909~011~+ : 65': 01 : 96- 1 1 -8~.: 10 ~13H0~ Vd~ 10~ 0~
~ 2 1 9 9 o 1 9 ~-~.r~3~3~
~0
: .
~x~un~le ~
T~e ~o~lowl~g ~orn~ iotls wer~ ~repared by mixing tho
d~e:~s~ ~ c~e ordor lis~ed.
,
~ hA~ON ~ by we~ht ~ ~ 4
Wa~e~
Ci t~ic ~cid 7 7
Z~oli~e 18. l~
P~lymer 1 ) 1. 5 1. S
10 Spa~ ~5~ 5
P~c~lve~; 6~ 33 . ~,3 .
5e~aLraeioz~ (in mm)
la~CB~ ~ weok~ ~c ~ O
ial Yi6cosi ty
(cp at 25C'C a~ 21/sj 146~ 2:50
sc~s~y Dri~t 540
~p a~tex ~ weelc~) .
S ~ Sor}~it~n trlolea~e, ~x :~CI
~0 6) ~re:a~x a~ $n B~le 1 wit,~ a ~ Ag r~ ,Ra~ 80:20
rrhi~ ~x}; ~r~e~t shows chat p~o~uc~ f'or~ tioD,~ ~T th
~ta~ w re~ Y~coslty ~ ts.
S ~ 3
Th ~ollowi~g ~o~ t14~s Wf~ prepa~e~ by m~x~ th~
~3gz edienc~ ln t~:e o~der l:l~tod ~
~ORM~T~r~N ~ Wt 1 . 5 6 7 a
w~c~ ~o 1 oo
3 ~ C~:t~lc ~id ? 7 7 7
~aoli~e ~8 ~ 13
Pvlym~r 1~ 1 . 5 1. ~ ~ 2
Stabil~er* 2 7) 2 8) . 4 ?l 4 ~)
Active le~rel~ 9,) 3i 3'~ 31 31
!~, a
A~EN~D SI~EE~ ~ I
WU '~ tJb',1!1 2 1 ~ ~ C i 9 . ~4r~w~
2~
~pa~ ~Lt~o~ ~) 0 ~
I~ie_al ~i~co~l~y
ti~ cp a~ 25~C
at 21~) 14ZC i430 1770 17~0
S ~ cosi~y r~ri~
, C~ at ~,5
a;~t~r 4 we~k3
ac ~ 2 ~0 2~0 250 27
.
lC ~ T~ese ln~e~;ts ~e~: a~ded as a p~ani.x
7~ Span 85 ~hich i~ it~n trio~aa~ ~}~a ~ x ICI
~ ~p2~ ~ which i~ ~ox~ita~ mo~olaura~e (HLB 8.6), ~c ~C~ :
9) ~r~Fix ~co~dl~ to ~c~ e 1 ~ a 2~t~ ei~ ~la
w~ 8~:2~.
Al~ fo~rnulatios~ Y~ l8~;7g the ~tabillser shaw sood
stabili~y, ~ow ~sco~lty ~ a ~ow viacosity ârif~.
Exa~lRLe 4
The :Eol~ow~ o~ulacix8 wore p~ a~d ~ ~ the '
in~redl~:at~ the order listed to wate~.
FO~ATION ( in ~wt ~ ~ 10
Water b~lan~ ~ ~A
2 5 Cl~lc Acid 1~ 1~
Z~oli~e 13 . 3 ~3 . 3
PCP 1.5 1.5
9tab~ er~ 2 ~ 0 10
Acti~re level ~ 33 3 3
~0
~opara~i~n
~a~e~ 4 ~e~ks i~ 4
~lsc3si ty d~i~ t
C 2S4C at 21/B1 ~8a lBO
35 ~afr~r ~ woek~ t)
AMENDED SHEET , .
~ ~ . t I . A ~ _ T T ~ -- . T A
W~ UO~ 9d r~
T~ese ingr~dien~s wo~e addea ~ enlx
~een a~, S~r~itaJ~ ~lo;~olau~ate, ex ;~C~
11~ P~a~ rl~ 1; NX~ ig~t ra~o w~ ~0:~
5 Althou~h ~Ot co~pl~tely co~ara~le, t~ ~rr~ a~cion~ with
~h~ a~ablllse~ has lowe~ D~lpl~r2~tiO~ a~l lower ~iaco~ty
d,ri~t llpon utora~e.
l Thi~ stra1 e~ ~he be~e~t o~ ~0~ ~he3~ a~ ~he
uEe ~ ~xic~u~ st~bili~er~ in sta~ atio~ u~ ~igh
;c ~o~ o~:s. ~he com~6i~io~ w~ p:~p~e~ ~y
~dding ~he i~g;~dient~ in the c~e~ l~c~d a~ a, t~.~r a~re
15o ~ 5 0 5 ~ C .
POR~ ~ N 11
Wate~ tO 100 to 100 'CO ~t~O ~0 100
ICO~ ) 16 . 71 16 ~ 71 '1 6 . 7l 16 . 7~
citr~c ~c~ d 9 ~ . 14 9 . 14 9 . 14
~0 Glyc~rol 4.17 4.~7 4.17 ~;.17
~oruc 2,~2 2.92 ~"~Z 2~92
So~ icarbon~to 3 . 5 3 . 5 3 5 3 - 5
~e~ e 4A~as lO~) 13 . ~3 13 .~3 13 . 3~ 13 . 33
~oly~er A~ 33~ 5 05 S.05 5.05 5.0S
~5 ~AS a~ 6 . 2~ 6 ~ 2S 6 . 25 6 . a5
9Y~t CrU~C ;~ 3 . 33 13 .33 13 .33 13 . 33
S~rA~ A7~ 13.33 13.33 13.33 13.3~
Stabili3er~ ~on~ 2~ ~P ~5 ~ 'rW 20 2~121 ~ :
~OO~ tO 30C 7~ 10) 12)
~0 ;P~LrU~ 4 . 0~4
'
p~ g.1 9.1 g.3 g.3
.~a~ Kt~ ratic~ 1.2 1~ l.Z
~h0~2 1~g~dlon~ were adde~l a~ a ~:~lx
3S 1~) Tw~e~ 21 ~s so~l~a~ mono~ trat~ ~i'ch 4 ~0 ~U~5,
AMENOED SltEET
C3~b~ ~Q ~ QT~(~171~T T~ : f)f): i l ' ~f~- l l -Q7~ H~N~llli\l Vd~ NOA ~
WO ~ 6~5 p~ J,"5J ~
~1 2 1 Y90 ~ q
Un~h~ d
';;~i'CJ Al ~iscosity ~sr~a~l) 1250 ~990 ~949 14sa
Y13co~ity ~4~ a~ ~a~ ~ 1420 18l30 ~060 ~ 14qO
Visco~i~y ~4iW at 50C) 1700 ~350 2300 ~ 0
.~ean se~ ur~ng A W 20~C ~.2% ~.2~ 2.0
Mean 3epn. d~in~ ~W 504C ~.6~C ~.0~ ~.8~ 3.4
Pc~ ~ d~
0 ;~n1~ is~o~ity ~mPa~ 1330 20~0 2~0~ 14
Visco~ity ~4W a~ 20C~ 1550 '690 ~010 125~
Mean sep~. 4ur~g q W ~0C z~ zero z~ ze~o
M~an sepn. duri~g giW 5~4C ze~o z~ro zero z~
~xtru~ pla~tometer use~ ~o del~ r a ~h~r oif
10, 00~ ~c~
~xample 6
~0 1~ pro~rides an ex~:~ 5~ high ~o~io~ic ~o~il ~ti~n~ d
~11UOE~r~S the be;s~e~it3 o~ the pr~fi9~ o~ ~ol~d ~a~t~cle5
a~ u~ o~ po~ s~iear. ~he c~~ Q~ 4n~ were ~re~re~
~y adding t~e ingrediant~ he ~2~der l~ sced at
tempera~u~e o~ SO~SX~C. Apa~ o~ the ze~l~te ~vel~,
25 E~ ul~io~l~ lS an~ ~6 a~e eq~ilra~nt, ths ingre~l~ e~to
comp~ c102~ 16 are ~resen~ ln che ~ io a~ in
composi~on 15 .
~o~ l atlo~ 15 16 17
.
l~iY:S9~ hf~. hR f~+ l ~Rl~ l [~+ ~ [I : '~h-ll-R7~ 10 N~H.'~N~iiW VH~I NO,~
W0 Yti~002~ Z 1 5i 5~G 1 9 ~~v.J~D
32
.
Wator t,o ~00 to 14a to 10
X~ 490 21.43 16,92 ~ a
Cit~ic ac~d 10 . g7 9 .14 S .14
Glycerol . 5 . 0 . ~ ,17 4 ,17
~4~ . 5 ~ . 9~ ~, g~
S~dium 13lcarbor.ate 4.0 3~33 3.33
Zeo~ite 4A l~s lC0~ - 13.33 1~.33
~olyme~ 33~) ~.06 5.05 2.S3
0~ acld ~ .5 6 . 2S ~ .2S
~0 Synp~ro~c ~ 6.0 1~.33 13~33
S~per~nic A7~ ~ 13.33 ~3.33
Sili~cne an~i1'o~m 0.2 0.17 ~. 7
p;~ 10.3 10.5 10,4
lS 2~a~:K~ ~ario 1:~.3g 1:1.15 ~:1.15
~nshear~d
iaL vi~c~ y ~*a~ s 1~8S ~ ~0
cosi~y ~4W ~ Z0C) 605 13~0 ll~a
- Vi~ 05i~;y ~4W at 50~C~ 4~0 1~0 1~94
~0 Me~ 33pn . - 4W 20C 1. ~ Z~ro 1.0
Me~ ~ep~ W 5~C 10~094 0.~ 1.29f
PC1~3t ~he~r~
~nlria'~ visccslty ~mPaa) Sl4 14~0 8~0
~iY~o~ 7 at 20DC~ 6~0 1360 ~200
as ~o~n ~epn. - 4w 20C zero ~r~ zera
Mea~ 3eF~ W 50C zero z~ro Z6~0
~xt-rusio~ pla~tometer u~;a~ ~o deli~e~ a 3he~r c~
10, ~00 3ec ' .
3 0 E~a~l ~ 7
Thas illu~t~t~ t~ be~its o~ ~siP.~ high~r Jol$:1 1~ol~
in a hish ~ ior~c SormLllatio~.
Th~ con~posi~lon~ we~ prepared ~y ~At~J he~ r~d~e~t~
: ,
.
.
AMENDED SHEET
3 3 9 1 9 ~ ~;3P5~
,.
.
the ~rder ~isted at a cemperatu~e o~ 50~S5C.
ion l ~j ~ 9
~a~er ~o ~00 t.o 1~0
~COX t~ .27 ~a.27
C~t~ cid 7. 0 7 . o
~;ly~ 7
Borax a . 5~ 2
Zeoli~e ~A ~as 100~ ~5 . 5 la . ~
Polym~r A ll ~33~) ~.OS~ 5.05
~AS acid~ . 6 . ~5 6 .25
Sy~p~r~ic A3~ 13.33 ~3.33
syDperonic ~7 t 3 3~ ~3 . 33
Sp~ 2~* ~.0 2.
~ 00~ c ~ 3 0 C
P~:rf~me o . 4 , o . 4
. .
pk~ 7.9 ; 7.9
:c~a~:X~ ratlo 1;1,~5 1:1
~ The~e ~ red1ents we~e add~ h~ ~om~ o~
~he~r A
Irltia~ visco~ ty ~m~a~) 990 1190
~lsco~ity t4~ a~ ~OCC) 1180 1g30
Vtscosi~y (4~ at 50C~ 1660
Masn ~op~4-Y ~0C 0~8% zero
~5 Me:a~ ~~ 4W 50~C 1.~ zero
~'he cocnpo~ition ~a~ shear~tlth a~ ~L plas~ome~r
at ~ shear ra~e ~ 10, Q00 6ec '.
~, , ' , ".
~;c~pL~ ~ '
30 T~ foll~wing exa~l~ non~trates c~t ~c~t-~h~z c~z; ?l~o:
be ~ cti~ using a de~ic~ which ~o~ pr~cticAl ~o u~
i~ 2ac~o~1e~ ~ namely a ~he~ . 'rhls wa3 a ~ ra~n
Y~ ~e - c~ æ~hr~ i3 scr~w~d, do~ u~t$1 ~ suic~ly
n~r20w c~3~ric~ c~ a~h~ad.
3 5
AMENDED SHEEJ
...,.. . ~. _..
C'~ ~ OC~C', C~ C~l ~ T.OTI~ T TC' ' ~ ~n ~ I T ~ _ r T _O~ Tn ~ au--U~ IW ~
r";,~ 38
3~ 21990i9
'rh~ ~mpo~cio~ we~e p~pa~ed ~y ~ n~ g~e~ien~3 in
~n~ or~r li~ d a~ a~ t~0~a~u~ o~ 50~55~.
F~n~ul a t t,~n 2 C
Water to 100
K0~ ~49~) 16.71
Cit~ic acl~ 3.1~ .
Glyc~rol 4.1
3~ x 2 .
1~ Qo~u~ bica~bq~a~e3.5
~ec~ e 4~ ~a~ 100~ .33
P~ All ~3.~) 5, 05
~AS acid* 6 . 25
Synperonic A3~ 13.33
lS ~;y:~e~ ~7~ 13.33
gp2~; Z4 ~ 2 . 0
Co~l ~a 3a oc
P~
9.1
2~ . .
~ The~e l~redi~t~ W~ added ~n ~h~ for~ o~ a p~emix
~ .
The ~or~ulat~on was either s~re~ a~ 20aC, or ~;ittY~ ~;0
I;;o~-sh~a~ ~y usi~g a shear ~ e~ o wcx~:-
~I0~ 2, ~3,
snea~ d~lce ~?one 5hear ~1~ Sh~a2~ Yal~r~
~ack p~es~ure ~ 2 ~a~ 7 ~ax
In~ ~lal ~1~3~031ty 15S0 1580 1~0
wsf~k viscosit~f 17~ 16~0 1540
w~c sepa~a~on 1~ zero ze~a
.
~hls example show~ .t~at post~shea~ h a shear-~ralve
3S improYe~ the vi~cosi~y ar~ ablli~y c~ar~c~erlæcic~ o~
liquid de~erge~t ccmpcsit io~ .
, AMENDED SHEET
~ ~ c~r~r~Q7~ r~Q r~ ~Q T C~f~C~ T T C~ T T qf~ ~ T T - Q,. ~ T ~ ~nw ~ AO~I
WO~J~ 2 1 ~9V i 9 rc~lr~l~
~.x~ ole 9
m~ ~ollowin5 li~:t~d W~L8 ~reF~ d ~y ~ the l~re~ie~
~n ~h~ order 1~ ~ e~ while keepi~ e tamp~ratu~e a~ clo~e
co 50~ as poss~ rhf3 acti~e~ w~e atde~ a~ Y. Th
~ulation was cooled ~o 30C ~e~oxe a~ ion ~ p~r~uma.
;
P~O~ A,-~ON
Water 6 5~ :
KOR ( 4 ~ ~ 3
10 Cit~lC acid
~;lycerGl ~ ~.7
~orz~x z .
Sodlu~a b~carbonate 3.5
Zeoii~e ~A ~0~ . 57
Po}y;ner ~ ~33~j 5~05
~,in~a~ ~lkyl i:~e~ne sul.~hon~d~ 6 . 25
Synpero:~ic A3~ 3.~3
Sy~ronlc ~7~ ~3,33
S~an 20 ~ox~tzLn mo~ola~rate~ 2.0
2 5 eer~u,ne 0 ~ 4
,
i~ palS~m~r ~ g ~crl~ed in 2P 34~ 995.
* Those i ~edi~t~ ware a~ d i~ the 20rm o~ a proQll.x
25 3ampl~s c~ the li~uid were pasacd ~hrough ~ tru~lo~
pl~s~on~erer. The reerul~ w~e:
~o~t she~r ra~ ~ioao/~ec~ -
a s ~ 3~ :
o~ weo~c~ sepn .
- (20 ~ C1 Y~ es ~ No ~o ~ Jo
weel~ ~epz~
~ ;O dagC) Y~s Ye~ o ~g ~e~ Yee ~ - -
3 5 4 w~eks moa~
~2~ 70~ 166~ ~7~ 1614 1130 1160 1~50
.
,
AMENDED SHEET . : .
9*#:S9**66~Z 68 6~+ ~*81909*01 1~+ : Z0:11 : 96-1~-8Z 1() ~3H~N3.1~ Vd3:N0,~
o s..i;v~ C .~ 3iC ~3 - ,~
3~ '
2199019
'~'h1Y eY ~ OC o~ly ~how~ ~hat ~7lying p~t-~hea~ to;
~ish ncnion~c llguid~3 i$ ~e~ic~al a9 it ~C~U~#~
aration ~t 20C. :Por t~ o~tl~n there ap~ears
op~.imum po~t shea~ rare aro~d IO,U~ ~oc~pro~al
3çaco~d~ a~ p~ysical R~a~ility 1~ achi~red with lit tl~
ch~e ~n ~rl~co3ity. t~ er~lly, ~ o~ti~um d~ ee o~
~ar ~ e ~rmul~o~ d3pendent a~ can ~e ~tabllshe~
~y exp~ime~ fo~ any given f~r~ulat~
e 1 0
~ormu:L2~ion 24 o~ ~x?s~le ~ wa ~ p~pa~ 3~p1a~ o~ th~;
~ id w~re ~a3~d throu~ ~n diap~r~gm 3hea~ e. The
r~~ul ~ ware: - .
~hear ~alve
Un~hea~d Low ~hea~ a ba~ ~igh ~h~ar~7
~0 ~atch 1
Sep~ ~0~) Ye~ ~o . ~o
~ea~ ~isc ~6gO 15Z~ 1513
~a~ch 2
25 S~n ~2 0C) Yeg Nc ~o
M~ 15~0 14~ 13~0
It ca~ be ~ee~ r ~pplica~ o2 pos~ shear, thi~ o
~ia u~e o~ a shear ~ e, ha~ coif~rr~di phy~ical ~cabll~ty
wi~ relaei~e~y little ~ang~ in ~cosity,
'
D 1~
~r~e ~ol~owi~ formNlatio~ w~ r~ar~:
,
AMENDED SHEET
V !~ Ub '1~ p~
37 2199019
F.'O~.~tJI.ATION ( ~ by Wf~ ' yht ~ 2 5
.
K~W~ 8.1
S~er~;Lic A7~ 15.5
~y2~pero~lc A36~15 . 5
~ycerol 4 . g
~o~ax 1 Ca~ 3, 4
2C~ cicra~e 4ag 12 . 4
Polyme;~
10 Wat~r 3~.
, .
I ~a~: K~ ~a~lo 1~ 9 .
15 ~or;n~la~ion 25 c~ntA~n~ ellar d~let0 t~at lack
i r.t~rn~ 1 symneery a~d cor~ain ~n~ co~e~tric 3urfac~ t
macerial.
E~ca~rDl3 12
... ..
2~ ~h~ foll~wir~g ~tl~ w~ arod:
~ . .
FO~tJI.~ hy wF~lght ~ 2~
Priolene 6902 6 . 09
~pe~ 7~ l2 . 9a
~5 ~ynpe~o~$c A~ 12.98
G~ ycerol ~ . 06
30rax lOa~ 2 . 34
, XO~ (50Pf~ ~.15
Na- carbonate 3 . 25
C~ tric Acid lag.g ~7
Z~ol it~ 1~ . 2
Po~yme~ ~ . a
Waeer & m~no~s ad ~00
- ; c
3 5 p~; 5 a4
N~ ti~ 2; 1
'. ' ','. "'',''';
AMENDED Sl IEET
J 17ft ' q~-i7~2~7~ ~S? f~i 171 bQT~\~ l 1~ : ~O: T T ~ T T ~ : T O ~ H~nw v~ IOA .'~
7~ 3G,~ 2~ S~J
21990l9
~o~l~tion 26 cvntains la;.n.ellar drople~s ~hat lack
ir~q~al s~:~nser~r a~d co~taln no~con~0~txla Yur~acta~t
mar e~
~le 13
'rhe ~411~i~ ulation w~Ls ~ are~ by pr~rrl~rin~3 th~
3ulfats and noz~ ic aLnd a~ thiE prer~x t~ a ~olu~o~
t~te, ~rat~, ~lyc~r~ e ~lymer. ~e~ t~
10 ~he ~ tur~ ~irred ~ith an ~oad ~ re~ ~or 30 minu~e~
a~ roo;~ mpera~4r~
rr~gr~d~ enc~: . ~e~ ~h~ %
50~ eco~ y alc~hol 3ul~te 1) 20
Nonionic 2~ 20
Sodlu~ citrat~ dihy~ra~
Sodium ~etz~2~.bo~a~e decahydra~e 3 . 5
Gly~e3:a:L 5
Poly~ner 3 )
Water tO 1~0~
~scosity 4~ 2~0 s~s
1) Avera~e ~tal alk~rl chai~ 16ngt~h '~5.2, ~otal ~ d 3
Z5 ~so~r coslte2~t 2
~) C1~ 13 ethoxyla~ea with 6.5 EO o~ a~re~a~
3 ~ Polym~ o~ A; 1 o~ EP-A- 0, 346, 995
w~ed wi~h a Haak~ consta~t~cr~s t h~am4~0r at 21~`
30 The ~ox~mla~Jo~ was ~u~led ulld~r polari~e~ l~g~t
icro~c~py and ~ ~alts~s ~ro~e~ w~r~ iden~i~ied. 'rha
liquld con~a~n~ dropl0c~ h a 3~1zo ~n l~he ra~e 0~ 2~ZO .
~m; chese lack rhtial sytnrnet~; the joi2~ed ~hick~e~s ~ t~e
b~ yex~ ln the . droplets ifi a~aller ~han ~h~ ~adiu~ o~ thd
35 dropl~ 9~ tha~ 25%, l.e. l~s~ than al~out 10~, o~
radiu~; th~ d~pl~t con~ist o~ly cs a ~-w la~llar ~
~MENDED SI~EET ..
w~s~/1062s ~ J~ JJIlJ3~s
39 21 9901 '~
layer~ s ~u~d u~ir;g a ~ si~n ~ectro~ rnl cr~sc~ .
comp~#~ tio~ ~o~ high ~ ~xibility in i~co~o~a~ic~ o
i~g~edl~
5 Bxam~l ~ L~
Su~ itut~g ~e ~econd~ ~pha~ o~ thc ~ ion c~
~ le ~ ith a second~ ulpha~ ~a~ring ~29~ o~ ch~ 2
an~l 3 isomer~ ~atio of n~njont~ ~o ~o~Lr~
~lphat~ co~np~lsing at 13a~t 3 C-atom~ o~ ~oth ~id~ o~ the
.0 C~ts:1m ts wkl~h l:he gUl~hat~ ~rou~ 1~ a~t~cheA i~ ~ro~
72~2~) ~e~u:L,,ed ~n a l~uid wlth dr~plet~ ;;~t cc~ ge~
ella~ layers a~d a core com~?ri~ ncn-co:~¢ont~lc
2llar phase; the ~n~d thirkn~ o~ ~he ~ ye~s 1
b~twee~ 50 and 9g~ o~ the radiu~.
~nlq 1~
Ir~creasing ~he i~ l o~ ~he Re~9~ ~pha~ o~ the ~re
~or~ula~on ~22~ 2,3 i~ome~s) o~ Xx~ 3 to 27~r a~a
louering th~ nonionl~ le~rel ~o 13~ ~ra~4 o~ aon~ni~ ~u
20 ~eco~darJ alkyl ~ulF~ate ~ 16i~g at lezi~r 3 ~-atom~ o~
bo~h ~id~ o~ the C~at~ t~ wh~c~ the su~p~t~ grou~ l~
~ttached t~ m 35:~5t ~ul~ed ln a l~usd w~th dropLeta
that ha~e ~ull bilayer ra~tal ~y~etry.
., .
2 ~ P~
T~e ~c~ uid ~aa pre~ared,:
ty acid 6
n~ c 1 1~ 13
Ncr~i~n1c 2 2 ) 1~
3 0 Glyc~rol . ~ .
I~o~ax lOe~a 3
KOH ~50~
N~2C~3 3
Ci~ic ~c~ 10 . ' '
3$ ~boll~e 4~ 16
Polymer 3 ) 2 :
~A~N~ED S~EEi
A ~ ~A~ A~ ~ T ~ A T T ~ . T T . 1~` _. T T _ C~, . ~i~ - 7-- _~A~ A /~
wo 9~tU6~S ~,~,t,j~
2199019
Ancl~oarl ~c snzym~F~
Wa~e;c ad 1~
1~ Nollior.lc 1 is Synpe~onic A7, ex ICI
2 ~ ion~ c ~ ~s Sy~e~onic ~3~ex IC~
3) Poïyrner All o~P pjP 3~6395
4 ) ~ bou~
T~.e li~uid did not. 6~0w phase se~ra~1o~ ~urlng 5 w~e~s 3t
37UC. Th~ tropl2t~ in t~e liquid s~ow~d n4 r dial syr~
At ir~rea3i~y po~yzne~ conce~ t~ons, ~he d~o~ 6 bocc~ 11
sc~1le~, Th~ ~n~y~ ha~.~ l.Lvo i~ h~ gh t~Dto~ la~ge~ ~h~
10 wee3cs ar~d 1~ ~a~c 5 w~el:s at 37~C) . 9~a~ y ~ g ~rur~ilor
i~cr~ased i~ po~c ~hear i~ ?lied, lr higher ~olymro
l~vel~ ar~ used and 1~ zcolic- level ~s in~r~a~ed,
i
ExamD1 e 17
T~e ;eolïowi~g lig~id was p~epar~d. Post 8hear ~d3 aF~li~.
:
Ol~c ~.C.i~l 7,5
n~
~0~103ic 2 2 ~
aï s
~5 30rax lOaq 3.5
XOH 150~ to plI o~ 9
Na2C03 4
~o~ymer 3 ) 1. 5
cit~ic a¢i~ 7.1
30 5~zyr~es
er ~& ~ s) ad 100
1~ Nonl~nic 1 is Synpero~lc A~ ex ~C~
n~ Syr~ronic A~ ~x ~C~ -
35 3 ) Polym~r All o~ ~P 345g95
The lic~u-l d co:ncains d~oplsrs t~at lacX ~dial s~
: .
~DED S~EET . . .
6JI06~ ;r~oh~ s
2~ 9901 9
E~ca5rrpl e 19
Th~ follcw~ny ll~uida we~ e ~y ~ 301~ g the alXa~
water, ~ trl~ ~h~ yl~c~c~r~te, ~he borax, t~
,po:Lymor a~d tha ac~l~fe ~r~x, wh~3~ x the mlx~u~e was
5 ~ d:
Co4~o~ition
"naF~ien~s . ~; ~y w.e,t~t .
Na ~ L~S 7 . ~
10 ~onlo;~ic ~. l) 15.8
r~O~ nic 2 Z ) 15 .
Glycsr~l 4~
~o~ax lOac~ 3,5
~a~ cl~rate . 2a~ g . g
15 P~:Lymer 3 ~ 1. 0
~t~r a~ lo~
1 ) S~peronic A7~9 '
) sy~p~ror~i~ 7~ -
3) :~olym~r Ali ~ E~ 3~6,~95
Cornpc~ition 2 w~ ~d~ by ad~liny ~n top o~ co~o~it~
20~ ~y weig~ o~ z~s~lir~ ~A m&ter~o.1, ex ~ a:L~t~ P (adde~
duri~ p~ap~ra~ ore the 0~ti~ p~x).
C~oqitio~ 3 w~ made bsr ~ ;a~ ol~msr to l~he
con~o~ n 1 ir.~ead o~ l'f by w~g~'c.
~ornpo~i~1~ 4 wa~ m~de ~ ~A~1r~ ~ c~ poly~er ~o t,~e
30 co~poaltio~ 9tead o~ y weisht.
C~rnpos~tlon 5 W~ macle ~y ~di~ ~ c~ polym~r to the
ccmposition 1 i~stea~ O~ y wei~ht.
35 Th~ ~o:Llowin~ r~sul~s were o~ta~ :~o~:
~AM~NDED SHEET
WO q6llV615 ~ 1 9 9 fJ~ T~ ua~l~x
42
Corr~o~it~ c~
3 4, 5
1 woek: -
Pha~e ~e~ar~ion 27 O 9 ~ o
Vl~co~ity 90 3~ ~S5 ~7~ 8~0
mqn~:
~0' Phage 5~3pA r~ n 3~ 1 0
~isco~ ~y 105 333 142 6~6 ~37
1~ !
I~ ~a~ be co~cluded ~at ~tAhll~ty ~cr3a~-so aD,dJor
co~lty improves ~ h a~ditio~ o~ solid particles a~ o~ .
by addir~g more polymer.
~5
Li~uLd compo~ ns 1-~ c~ta~ ~rople~ t~ ha~ a
ctu~e l~k~na i~e~ 4t~y.
Comp~ltlon 4 d~E ~ ~how no ~ha~e q~parat~l~r~ a~t~r ~ ~
20 w~ek. The c~ lo~ ~a~ c:e~rl~u~ed an~ the 2~cli~
r~;wed, wherea~ter ~he x~s~lti~g L~4id W~L9 r~ . ~e
r~xed ~oznpo~it~on t~hi~h i~ e~u~l ta c~ ~Q~iric~
~hodred phase ~oparz~t~e~ after ~ wesk s~orage s~m~ to
cornpo~itio:~ 3. ~t ca~ e ~:on~ ded t~t ~~^nr-9 o~ solld
~5 ~art~cles in~rease~ stab~ lie~
: ' '
Fxan~ 3
llow~s ~quid w~ p~e~reds
~n~re~dlgr~ts~ by we~ yht
3a ~cnion~c ~ ~ 13
Nonionic 2 ~ 13
,~S ~Cid 6 .
Ze~ e 13
Polym~ 37 ~.S
~:~z~ & st~ r~ 7
W~er ~ ct~olyte ad 100
-, . ,:
A~IYDED SHEET I ...... _.
W~ ~*~ ~J~;-;'.. ~r, '
2 ~ 9 ~ ~ :
Sy~p~o~ic
~) 5y~ero~1c ~7~
l 3 ) P~:Lymer All of' ~3P 3~ 5
9pan 20 ~as ~dd at ~riou~ la~d th~ ~llow~n~
3t;abllitie8 were o~r~ i~e~
~1 ( % by weiyht ) o ~ o~ 6 . S
Sepasation a~r ~ w~ ; 37C4.5 3,5 ~.25 3.~5
' ' ' '
il lu~t~a~es th~ ~o~ e~ec~ o~ 8pans o~ th~
~iscosicy o~ high nonio~ic ~ coslty d~i~t wa~ als~
i~?rc~ved .
1~ :
~camr~ 2 0
~z~m~ s~ y wa~ a~u~ed i~ the ~ or ~ 1e 19
~nd ~ound to ~ ~e~y goo~: 9a~ for lipa~ and 74% ~or
~ro~ase af~er 4 week~ t ~7
!
FY~P13 ~1
~a~ious le~ o~ ~olid E~a~cles w~e ~dded to th~
o~ :~xa~le 19 a~ the ~ollowi~g roaul~s ~er~ obtai;~od:
~5
Z~llte le~rel ~% by welg~ i3 15.5 18 ao
~eparatibp~ (4 wee~ a~J~ieD,~ 4 2 0 0
~iB ~hows th~Lt ~oli~ pa~lcl~ c~ sta~t l~s~ hi~h non~o&~c
30 l~ e ~a~ne co~o~Sio~ wi~oue sali~ partic~es
s~owe~ his~ sep~a~l~P, aSte~ ~ week~ a'c a~ient.
F~,~le ~
3~ I~h~ l;Lgui~ c~ ~xamp}~s 1 and aI a~ 2X ~ ~P A ~ 0 w~e
prepar~d .
~ÆN~L~ T
A~-IAAL_A~ ~A T ~ A T T ~ . . A~ . ~ ~ ~ ~A~ A A --.Y
W~ 2~ , ~j~,~,~;
219~0i9
2xa~:Le 1 resul~ad in a liquid whieh, wher~ ~tu~d und~r
th¢ el~e~o~ ~e~ eF~, ~wa~ ~aund to e4~ain ~t~r~aeta~C
droyl~ts ln ~n i~otropi~ $~uou5 pha~e. ~ u~aetarlt
~r~plees al~ ~t ~ow ~r~i3gent und~ the elec~r~
5 mi~r~cap~ tUds~ o~ the dro~l~t~ w~ fx~ze-~r~ct~c~
~lec~n m~cra6~0py ~ev~ealed t~t che ~urfae~t ~xopl~t~
hD.~ ar ~rati~g o~ the outside and stacks of
t~nt in tho co~e. The level o~ ~oLld ~a~e~cles wa~
e~tirca~ed t~ b~ ~ut 5~ by w~lght o~ e co~o~it~,on,
- 10
'rh~ ; 0~ Elx~ 9 Z:~ an~l 2R were ~x~a1r~d a~d they ~¦
were st~d~ed u~der th~ elect:ro~ micrcscope ~L~t f~nd ~o b~
cotnplete sp~eruLite~.
AMENDED SHEET
