Croda Home Care

Presents

A Formulators
Guide to
Emulsification &
Solubilisation

1st/2nd March 2016

Innovation you can build on

Welcome
During this webinar series we will explain and guide the
formulator through the challenges faced in making choices for
todays formulations

Formulation Practical
Challenge
Design Solutions
 Croda Home Care
Presents

The Story of
HLB

Innovation you can build on

Why use the HLB system?

Ill use what Ive

always used

Ill ask colleagues Use the

what theyd use
Or HLB
I think this will
System!
work

Id best try
everything
 Tell me more! What is the HLB system?
Surfactant Hydrophilic Lipophilic

More Hydrophilic = Higher HLB More Lipophilic = Lower HLB

System is designed for non-ionic surfactants

HLB is the Hydrophile/Lipophile Balance
 Tell me more! What is the HLB system?
Surfactant Oil
Hydrophilic
Lipophilic

HLB Value HLB Requirement

Each oil or application has a particular HLB requirement

If HLB Value = HLB Requirement Good Performance

OK, so what can HLB help me do?
OK, so what can HLB help me do?
We can help!
 Croda Home Care
Presents

HLB the
Concept in
Practice

Innovation you can build on

 The HLB System
HLB = Hydrophile Lipophile Balance

Lower HLB, more Higher HLB, more

Lipophilic (oil soluble) Hydrophilic (water soluble)

HLB 4 HLB 15
Span 80 Tween 80

Home Care
in water: in water:
Why is this Useful?
Non-ionic surfactants have HLB values how
water or oil soluble they are
Oils have required HLB values the HLB
needed to create an emulsion

For example:

Home Care
Surfactant Oil
HLB 10 Required HLB 10

Stable emulsion
The HLB Kit
Is a simple, practical technique to determine the required HLB of
an oil

It is particularly useful for oil in water emulsions

The kit contains 8 blends of emulsifiers across the range of the

HLB scale

You then create 8 emulsions and find the most stable one

At first, accuracy isnt too important as you can refine things later
on have a quick play in the lab to see what you get
 Step 1 Make an HLB Kit
Ingredients: Span 80, Span 85, Tween 20, Tween 80
Blend into 8 small jars as follows:

HLB 2 HLB 4 HLB 6 HLB 8 HLB 10 HLB 12 HLB 14 HLB 16

8% Span 80 83% Span 80 46% Span 80 9% Span 80

92% Span 85 17% Tween 80 54% Tween 80 91% Tween 80
88% Span 80 65% Span 80 28% Span 80 60% Tween 20
12% Span 85 35% Tween 80 72% Tween 80 40% Tween 80
 Why do we use blends in the kit?
You could try to make a kit using single products closely matched to
each HLB you wanted to test
However this is not advised we always use blends of 2 (or more)
emulsifiers in practice

Using blends has a number of benefits:

You can tune the HLB values to exact integers
You get better coverage by the emulsifiers at the surface of the dispersed
droplet (better packing at the interface)
Increased emulsifying power, similar to multi-surfactant cleaning systems
Simplicity fewer products to order!

Mix of high &

Single emulsifier
low HLB
 Step 2 Use Your HLB Kit
Firstly youll need 8 jars, (around 25ml is ideal)
Label one for each HLB (2-16)

Importantly
Add 0.5g of Add 1.5g of mix the oil and
your oil phase HLB 2 to jar emulsifiers Add 18g of
Shake them all
to each jar. #2, 1.5g HLB together water to each
up!
(Suggested 4 to jar 4 and This gives jar
starting level) so on more efficient
emulsification
Step 3 Assess Your Results
You are looking for the best result the most stable emulsion
It doesnt have to be perfect, just the best one
You may see it straight away, overnight, or after a few hours in an oven
If all look too good, you can reduce your emulsifier level

HLB 2 HLB 4 HLB 6 HLB 8 HLB 10 HLB 12 HLB 14 HLB 16

Step 4 Refine and Optimise
HLB also works for mixed oil systems e.g. in formulations or
when cleaning a mixture of oils/waxes
The blended mixture just becomes your oil phase

Adjust your water phase as well pH, water hardness and

temperature should all be changed as required

When you have your initial HLB you can refine to get a more
accurate HLB, choose the best chemistry for your emulsifiers and
optimise the levels required

Well demonstrate this with a formulation example

 Worked Example Silicone Polish
The unstable formulation with no emulsifiers

Product Functionality %w/w

10000/200 Fluid Dimethicone Film Former 2.5
CrodamolTM GTCC Film Former 2.5
OptasenseTM G81 (2% solution) Rheology Modifier 2.5
Water Solvent 92.5

Next steps:
Run an HLB kit
Optimise the surfactant system
Final, stable formulation
Assess Your Results

2 4 6 8 10 12 14 16

HLB 6, 8 and 10 have

similar stability
Refine Required HLB
Reduce the amount of Fill in the gaps for HLB 7
emulsifier to reduce and 9
emulsion stability and HLB 8 shows the most
highlight differences stable emulsion

6 8 10 7 8 9
Refine Chemistry & Surfactant Levels
Refine Chemistry Refine Surfactant Level
Span 80 / Tween 80 vs
Span 60 / Tween 60 Formulation was made
with reduced levels of
surfactant
80 60
Formulation no longer
stable below 2%
surfactant
Surfactant level in
formulation set to 2.3%
 Car Interior Shiner Final Formulation
Final formulation
a stable
emulsion
 Croda Home Care
Presents

Case Study
Industrial Plant
Cleaning

Innovation you can build on

Case Study Industrial Plant Cleaning
The Problem
Industrial customer has a plant using long chain fatty acids and
alcohols hard, waxy solids
Standard cleaning process led to residues in vessels & pipework
Contamination of batches meant expensive filtration steps

The Requirements
New cleaning formulation low foam,
low hazard, low cost, effective on a
number of similar soils, Clean in Place

The Solution
Design an emulsifier blend to give
enhanced cleaning with fewer rinses
Case Study Plant Cleaning

Top down view

Clean vessel Soiled vessel

Low Performance Hot Water Washing

Drain

Vessel

Top down view

High Performance Emulsification Cleaning

Drain

Vessel

Top down view

Case Study Plant Cleaning
The Results (after just one rinse)

64% clean 99% clean 91% clean

Hot water Emulsification SLES

The Benefits
Saves energy, water, time and money
One wash step as opposed to three
Low foam on plant gives easy rinse-out
Emulsification ensures product washes away fully, no residues in pipes
Prevents filtration of contaminated batches
 Croda Home Care
Presents

The Versatility
of HLB

Innovation you can build on

The Versatility of HLB
HLB can be used across a wide range of lipophiles

We want to spark ideas, rather than being too prescriptive how

could you use HLB for your cleaning applications and
formulations?

As a general rule of thumb, here are the required HLBs for

some common groups of oils:
Vegetable oils 5-7
Silicone oils 8-12
Petroleum oils 9-11
Ester emollients 10-12
Fatty acids and alcohols 14-16
Some Specific HI&I Examples
Whether you have an oil to emulsify into your formulation, or an
oily soil you want to clean, the process is the same

Lipophile Function / Effect Required HLB

Crosolv G Non-VOC, degreaser solvent 10
d-Limonene Degreaser, solvent 6-7
Mineral oil Solvent, film former 10 (9-11)
Argan oil Emotive ingredient from Personal Care 11-12
Beeswax Natural wax for polishes 9
Cotton seed oil Emotive ingredient 5-6
Emulsification Cleaning
Emulsification cleaning has many benefits
Low environmental impact
Low or zero hazard class
Cost effective

Ideal for:
Oily soils with simple composition
Occasions when redeposition can be an issue
Low foam or high agitation requirements
Fast throughput Industrial applications, Clean in Place

Less suitable for:

Complex, mixed soils
Inorganic scale, particulate soils
Industrial Kitchen Cleaning Cooking Oil
High levels of oil used in certain types of
cuisine are difficult to remove

Traditional dishwashing formulations are

effective at grease, not oil

Application of the HLB test shows the ideal

emulsification HLB for sunflower oil to be 4
100% Bio-based
HLB 4 APG SLES Kitchen Cleaning:
Traditional surfactants 88% Span 80
are unsuitable for 12% Span 85
emulsifying
cooking oils:

0.5% surfactant, 40% oil

Industrial Cleaning Biodiesel
Chemicals in the oil industry are used under
strict environmental regulations

Typical surfactants require high water usage

and can be hazardous to operators.

Application of the HLB test shows the ideal

emulsification HLB for biodiesel to be 6
Industrial Biodiesel
HLB 6 APG SLES Cleaning Solution:
Traditional surfactants 83% Span 80
are unsuitable for 17% Span 85
emulsifying biodiesel:

0.5% surfactant, 40% biodiesel

 Croda Home Care
Presents

Solubilisation

Innovation you can build on

What is Solubilisation?
Perfectly clear solubilisation is an emulsion where the dispersed
phase has a particle size small enough to be invisible

Common oils which require

solubilising in HI&I include:
Fragrances
Essential oils
Solvents, e.g. Limonene
Emotive ingredients
Skin conditioning agents
 Products for Solubilisation
Croduret 40 NatraGem S140
Ethoxylated Castor Oil Ecocert approved natural
Very low odour Counter irritant
Paste/semi-solid Particularly effective on
essential oils
Croduret 40LV
Coming soon!
Low viscosity version Crodasol WS
of Croduret 40 Excellent fragrance
solubiliser
Fast dissolution
On Cleangredients.org
Tween 20 or Tween 80
Traditional liquid
solubiliser
Very effective
 Solubiliser Usage, Optimisation & Choice
Premix your oil and solubiliser various ratios should be tested
Start with 1:3, 1:5 and 1:10
Add your water (again, this should be relevant to your formulation,
so include other formulation ingredients, adjust pH etc.)
Assess stability and optimise further
% Solubiliser required to solubilise 1% lipophile
Lipophile
Croduret 40 Tween 20 NatraGem S140 Crodasol WS
(HLB 13) (HLB 16.7) (HLB 14) (HLB 14)
Fruity 6 5 2.4 5
Peach Leaf 10 7 12 9
Tuberose Fabric 4 5 12 6
Limonene 15 8 4 3.5
Solubilisers Summary
An HLB kit is not always useful for solubilising oils single
products often work well

Effective solubilisers usually have an HLB in the range 13-18

Higher HLB products are often solids, which arent always
practical

Solubiliser choice typically comes down to balancing the

benefits physical form, dissolution, natural/green as well as
performance

Surfactants in a formulation for detergency may help also act

as solubilisers

Always premix your oil and solubiliser

Thank You for Listening
In this webinar we have shown a formulators
guide to:
Practical use of the HLB system
How to tailor this to your exact needs
Using simple emulsifier blends for highly effective
cleaning

Home Care
A range of solubilisation solutions

For further information or formulations then find

them on the Croda website
www.crodahomecare.com
 Croda Home Care
Presents

Appendix
Emulsion Types &
Characterisation

Innovation you can build on

Oil, Water and Emulsions

So you need to clean an You need an emulsion!

oil, or stabilise it in your A stable mixture of two or
formulation? more immiscible liquids
Emulsion Types
Primarily, there are two types of emulsions, defined by which
phase is on the inside and outside (or which is the continuous
or dispersed phase):

Oil in water (o/w) Water in oil (w/o)

Emulsion Types
The phase of the greatest volume tends to become the
continuous phase
e.g. 80% oil phase = o/w emulsion

The orientation of the emulsifier changes depending on the

emulsion type:

Oil in water (o/w) Water in oil (w/o)

 Oil in Water Water in Oil
Oil droplets stabilised in water Water droplets stabilised in oil
Disperses in water: Doesnt disperse in water:

Added to water Mixed On standing Added to water Mixed On standing

Most common type for HI&I Less relevant for HI&I

Oil in Water Water in Oil
Examples can include car wax, Examples can include aerosol
fabric softener, silicone polish, insecticides
dashboard polish, leather
treatments, degreasers
 Croda Home Care
Presents

A Formulators
Guide to
Emulsification &
Solubilisation

Innovation you can build on