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emulsions stabilized with anionic and nonionic surfactants indicate that the new method
can effectivelypreventpermanentphaseinversionin high-internalphaseemulsionsand allow LEE processingat higher ratios of unheatedphaseto heatedphasethan did the original LEE method. It was
discovered
that mixing time and mixer rpm aswell asthe bulk temperatureand the sizeof the withheld
phasehave significanteffectson the mean droplet size of finishedemulsions.
INTRODUCTION
358
centratepreparation
stageand a dilutionstageasindicatedbelow:
OriginalLEE
First Stage:ConcentratePreparation
Internal Phase(heated) + [e EC (EmulsionConcentrate)
SecondStage:ConcentrateDilution
EC + txe - Ef (Final Emulsion)
Third Stage:txi-PhaseAddition
E2 + txi ---> Ef (Final Emulsion)
EXTERNAL
PHASE
-x
359
CASEfA}CASE(B]
=0.33
INTERNAL
PHASE
--
!
......
(A)-
.........
(B}---
C.= 0.67
.e: 0.67
0.5
EMULSION
Figure1. Comparison
of twodoublewithholding
LEEprocesses.
In bothcases
internalphase
equals
one
thirdof external
phase;
oqandoe arewithheldinternalandexternal
phases
respectively;
[3,andIBeare
heated
internalandexternal
phases
respectively.
CaseB is moreenergy
efficient
dueto a largerwithheld
externalphase%. Splittingof the internalphaseinto oqand[3,andusingonly[3,for the initialemulsificationreducethe dangerof phaseinversion.
of the externalphasevolume.ForLEEprocessing,
theexternalphaseis predividedinto
withheldOL
e phaseandheated[ephase.If the divisionof the externalphaseweremade
at Oe/lBe
= O.33/0.67asin theCase(A), indicated
bya dashed
line, thevolumeof [e
phasewouldbe significantlylargerthan the total internalphaseand generallythere
wouldbe no greatdangerof phaseinversion.To achieveevengreaterenergyconservation,the divisionof the externalphasemaybe madeat a highero/[3cratio. In Case
(B) shownwith a dottedline, the OLJ[
e ratio is chosenat 0.67/0.33. This meansthat
A bettermethodproposed
hereis to divide the internalphaseinto oqand 13i.If, for
360
additionof an external-phase
fluid (oe phase)thereis little dangerof phaseinversion.
Althoughthe third stageoperationrequiresadditionof the remaininginternalphase
(oqphase)thereis no greatdangerof phaseinversion
sincean additionalamountof the
external-phase
fluid wasaddedto the bulk in the secondstageoperation.Hence, the
newdouble-withholding
procedure
effectivelyreduces
the dangerof irreversible
phase
inversionduring the manufacturingprocessand allowsLEE processing
at relatively
high o/ ratiosto achievesubstantialenergyconservation.
EXPERIMENTAL
RESULTS
AND
DISCUSSION
EFFECTS OF % AND %
361
---.Ir2 MM I--'-t-
IOMM
50MM
6 MM --4
as the oil-solublesurfactants
were initially placedin IBiphaseand the water-soluble
surfactant
aswell asthe water-soluble
polymerwereplacedin the IBephaseasindicated
in Table I. Mineral oil and deionizedwater were divided into both o and [ phases.
362
O/W
Emulsion
Wt.
Phase
40.0
3.0
2.0
Glycerylstearate
SE
Cetearylalcohol
Sorbitansesquioleate
[3,
1.0
2.0
0.5
[3
[3,
Triethanolamine
AqueousPhase(External Phase)
Deionizedwater
50.9
0.4
0.2
Sodiumlaurylsulfate
Carbomer934
Total
100.0
Table
II
O/.,O/'e 0
0
0.1
0.2
0.3
0.4
0.5
0.6
0.7
0.8
O/W
O/W
O/W
0.9
0.1
O/W
O/W
O/W
0.2
O/W
O/W
O/W
O/W
O/W
O/W
O/W
O/W
O/W
O/W
O/W
O/W
W/O
O/W
O/W
O/W
O/W
O/W
O/W
O/W
O/W
O/W
O/W
O/W
0.3
0.4
0.5
W/O
W/O
W/O
W/O
O/W
O/W
O/W
O/W
O/W
W/O
W/O
W/O
W/O
W/O
W/O
W/O
W/O
O/W
O/W
O/W
O/W
O/W
O/W
O/W
0.6
0.7
0.8
0.9
W/O
W/O
W/O
W/O
W/O
W/O
W/O
W/O
W/O
W/O
O/W
O/W
O/W
O/W
W/O
W/O
W/O
W/O
W/O
W/O
O/W
O/W
O/W
W/O
W/O
W/O
W/O
W/O
W/O
W/O
O/W
W/O
W/O
W/O
W/O
W/O
W/O
W/O
W/O
W/O
W/O
O/W
O/W
O/W
O/W
W/O
1.2
0.15
HIGH
INTERNAL
EMULSIFICATION
363
i!
.8
.7
o/w
.6
.4
.3
w/o
.2
= 1.2cxe-0.15
.I
-.I
-.2
.2
.3
z
.4
J
.5
.6
.7
.8
.9
holdingtechnique.
In thiscase,the smallerthe slopeof the line, thegreateris the
effectiveness
of withholding
oqin preventing
phase
inversion
to formW/O typeemulsions.
emulsion.
364
I
200
400
600
MIXER
800
SPEED
I
I000
i,
I
1200
I
1400
(RPM}
represent
a significantvariationin processing
conditions
and thusa largevariationin
the propertiesof the emulsionscan be expected.In addition to o values, emulsion
temperature,mixing time, and the rate of mixing canalsohavesignificantinfluence
on the final emulsion.
EFFECTS
OF MIXING
The majordifference
betweenthemodifiedLEEandtheoriginalLEEis thethird-stage
operationin the new techniquewhich involvesan additionof oqphaseinto the emulsion
concentrate,
E2. Althoughaddingoil into a preformedO/W emulsionmay represent
a radicaldeparturefrom a normallyemployedemulsificationmethod, there are no
theoretical
groundsto believethat sucha procedure
wouldnotproduce
a commerciallyacceptableemulsion.
HIGH
INTERNAL
365
5O
4O
= 27"C
3O
= 300
2O
RPM
I0
r-
=mmO 0RPM
R = moo0 IPM
0
o
I0
MIXING
12
14
16
18
20
22
24
:::)6
2_8
TIME, ,9 (MIN)
366
25
I0
20
30
40
50
60
70
TEMPERATURE
OF E2 , T (C)
__
OF TEMPERATURE
Temperature
is, of course,a very importantfactorin all emulsionprocessing.
An
exampleshowingthe effectof the initial temperature
of the E2 emulsionon the mean
dropletsizeof the final emulsionis shownin Figure6. It is interesting
to notethat
themeandropletsizeshows
a minimumat an E2 temperature
of about40C.It is
believedthat the existence
of the minimumpoint is probablydue to a viscosity
effect.
At a constant
mixerrpm, size-reduction
is mostefficientat a moderately
highviscosity
rangefora shear-thinning,
time-dependent
emulsion.
Ascanbeseenfromtheviscosity
datain Figure7, theviscosity
oftheemulsion
dropssharply
at around
50C,resulting
in a loweredshearactionby themixerrotatingat a constant
rpm. On theotherhand,
asthetemperature
dropsbelow40C,theincreased
viscosity
andtheyieldvalueprobably makethe mixinglessefficient,resultingin the formationof coarser
emulsions.
367
60
50
40
30
o
u
IO
IO
I
0
I
:30
i
40
tEMPEr/TUrE,
I
0
60
70
t { C)
CONCLUSIONS
Experimental
datapresented
hereindicatethat themodifiedLEEtechnique
canbeused
to process
O/W emulsionswith relativelylargeinternalphasesor to carryout LEE in
a higherot rangewithout encountering
the usualcomplication
of unintendedphase
inversion.
Althoughall experimental
datapresented
herewereobtained
onlaboratory
scaleequipment, somepilot plantwork on differentformulations
wascarriedout to demonstrate
the feasibilityof usingsucha technique
on a commercial
scale.When carriedout at
correctoti and otevalues,emulsification
proceeded
verysmoothlyto yield stableemulsionswith very fine texture.
unintended
phaseinversion,
ascanbe seenfromthe datain Figure3; it canbe used
368
The success
of adoptingthe method, however,may be dependenton properselection
of the sizeof oteand oti as well as the mixing equipmentand mixing conditions.As a
rule, oteand otivaluesshouldnot be selectedat points too closeto the phase-inversion
boundaryline.
ACKNOWLEDGEMENT
with
this research.
REFERENCES
in higl-'-zange,
Cosmetics
andToiletries,
95, 33-39 (December
1980).
(5) T. J. Lin, T. Akabori, S. Tanaka,and K. Shimura,Low-energy
emulsification
IV: Effectof emulsificationtemperature,Cosmetics
and Toiletries,
96, 31- 39 (June1981).
(6) T. J. Lin, T. Akabori, S. Tanaka, and K. Shimura,Mechanisms
of Enhanced
Emulsification
in LowEnergy
Processing,
Paperpresented
at 12th I.F.S.C.C. Congress,
Paris,France,September
1982.
(7) T. J. Lin andJ. C. Lambrechts,Effectof initial surfactantlocationon emulsionphaseinversion,J.
Soc.Cosmet.Chem., 20, 185-198 (March 1969).
(8) P. Becher,Emulsions.'
Theory
and Practice,
2nd ed., (ReinholdPublishingCorp., New York, 1965),
pp 101-104.