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,4. 80 60 1 . 0 Q

I

S 20

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A S * •\*5> 0.2 0.4 0.6 0.8

D isp ersed Phase Concentration (-)

A -450rpm # -600rpm □ -750rpm a -900rp m

Fig. 5.9. Correlation of Sauter mean diam eter, with Xylene Dispersed Phase Concentration, (j), at Im peller diam eter, Di = 0.05m.

240 1 E 200 -- 3 s 160 -- s E .2 120 - - I . . - u

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40 -- 0.6 0 0.2 0.4 0.8 1 D ispersed PhaseConcentration (-) A -200rpm ♦ -300rpm □ -550rpm ♦ -700rpm

Fig. 5.10. Correlation of Sauter mean diam eter, d]2 with Sunflower oil Dispersed Phase C oncentration, ({>, at Im peller diam eter, D, = 0.05m.

Chavter 5_________ ;____________________________________ Results and Discussion

The shift in size distribution to smaller average drop sizes for (j) > 50% was not clearly

distinguishable (cf. Fig. 5.8b and 5.8c). Figures 5.9 and 5.10 are a simplified

representation of Figs. 5.7 and 5.8 respectively. In these plots the different markers

represent the change in Sauter mean diameter with increasing dispersed phase

concentration for the four impeller speeds considered for each liquid dispersion system.

From the drop size distribution (DSD) plots it can be deduced that the average drop

size increases with an increase in dispersed phase concentration, ({) up to a point beyond

which further increase in the dispersed phase concentration causes the average drop size

to decrease. Although the results for sunflower oil are not clearly evident, these results

are in general agreement with the data reported recently by Boye et al, (1996) and

previously by Clarke and Sawistowski, (1978), Kumar et al, (1991) and Boye and

Ayazi Shamlou, (1994). The dashed lines represent the theoretical predictions of the

model postulated and once more seem to support these findings.

Experiments were conducted for aU three impellers studied and the results are illustrated

in appendix (C3.3/C4.3). In cases where there was excessive vortexing and air

entrainment the experiment was aborted (especially Di = 0.08 m). Clarke and

Sawistowski (1978) suggested that the observed change in the dependence of drop size

on the dispersed phase concentration was due to phase inversion which generally occurs

when the dispersed drops are packed closely in the suspension. Following phase

inversion the continuous phase becomes the dispersed phase and the dispersed phase

substituted by the continuous phase. Phase inversion is usually characterised by a step

change in some of the key physical properties of the two-liquid phase mixture, for

Chapter 5_____________________________________________ Results and Discussion

(Kato et a l, 1991). The type of emulsifier used in a dispersion has profound influence

on its stabilising or destabilising properties in addition to the hydrodynamic conditions in

the stirred vessel which ultimately determine the structure of the dispersion.

Matsumoto (1983) has described a method of producing duplex emulsion and dispersion

structures through thermal induction by assessing the extent of oil layer on the surface of

the dispersed aqueous compartments using a viscometric method. This method requires

measuring viscosity changes under glucose concentration gradients between inner

aqueous suspending fluid in order to estimate the area of the layer separating the two

aqueous phases. He also observed that the area of layer separating the two aqueous

phases mainly depended on the molar ratio of the polymer used (e.g. polyoxyethylene

sorbitan monooleate - Span 80) to the hydrophilic emulsifier in the sample.

Anionic surfactants such as sodium dodecyl sulphate (SDS) used in this study appear to

provide a wider molar ratio (4 60) than non-ionic polymers (polyoxyethylene sorbitan

monooleate - Span 80); cetyl trimethyl ammonium bromide (CTABr)) for the formation

of complex water-oil-water type (W/OAV) dispersions. To determine the formation of

global phase inversion, other experimental measurements such as the dispersion

electrical conductivity and rheological behaviour are considered in the subsequent

Chapter 5______________________________________________Results and Discussion

5.2.1 EFFECT OF DISPERSED PHASE C O NCENTRATIO N ON DISPER SIO N ELECTRICA L CO NDUCTIVITY

The data in Figs. 5.11a and 5.11b represent typical electrical conductivity measurements

and refer to experiments which were carried out at a fixed speed of 450 rpm for xylene

dispersions and 200 rpm for sunflower oil dispersions respectively. For both two-phase

liquid dispersions, several measurements of electrical conductivity were made for each

dispersed phase concentration as a function of time shown in both plots and for

comparison the conductivity of the pure dispersed phase and aqueous phase containing 0.3

wt% SDS are also depicted. The results show a gradual change in the electrical

conductivity of the dispersion with increasing dispersed phase concentration, but there is

no evidence of a sharp change in the conductivity that can be associated with the

phenomenon of global phase inversion (appendix C3.4/C4.4).

These results are contrary to those reported by Quinn and Sigloh (1963) and more

recently by Brooks and Richmond (1991) who observed a sharp change in electrical

conductivity. Moreover, visual assessment of the vessel contents showed no significant

change in the colour of the dispersion as dispersed phase concentration for both systems

increased. In most of the experiments, the mixture had a shiny appearance, characteristic

of an aqueous-continuous phase dispersion. In a few cases however, especially those

involving very high dispersed phase concentrations and speed of agitation, the dispersion

became dull in its appearance. In these cases, it was not obvious whether the change in

colour had occurred as a result of phase inversion or émulsification. The results from these

experiments were excluded from further analysis. Additional experiments such as

rheology measurements and visual assessment of the dispersion were performed to

Chapter 5 Results and Discussion