Dr Ian Maxwell
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HYPERDISPERSANTS INHYPERDISPERSANTS IN
NANOTECHNOLOGY APPLICATIONSNANOTECHNOLOGY APPLICATIONS
NanoMaterials 07
1st May 2007
Ian Maxwell - Noveon
© The Lubrizol Corporation 2006, all rights reserved
OUTLINE
• Nano particles / properties / stabilisation needs
• Overview of Hyperdispersants technology
• Solsperse product range – how to choose
• How to use dispersants – milling or surface treatment
• Noveon TS and Development Capability
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• Working with particles with sizes between say 5 nm and 100nm
• Working with giant molecules that have some defined shape
– Buckminster fullerene (“Fullerene”)
– Carbon nanotubes
• Molecular Electronics/Molecular computing.
– Processes happening within a single molecule
• Microengineering
– Tiny machines (actually micron, not nanometre sizes)
– “Nanobots”
WHAT IS NANOTECHNOLOGY
Only the first named area probably has
any interest for Noveon Hyperdispersants
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Some “nanoparticle” products
5 nm 100nm50 nm
Conventional tinting
pigments
Transparent pigments
Iron oxides, TiO2 based UV absorbers
Ceramics
Sol gel processing conventional/grinding processing
“Quantum Dots”
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TYPES OF NANOPARTICLESTYPES OF NANOPARTICLES
MAGNETISMIRON OXIDE
CONSUCTIVITY / MECHANICAL STRCARBON NANOTUBES
CONDUCTIVITY / IR ABSORBANCEANTIMONY TIN OXIDE
CONDUCTIVITY / IR ABSORBANCEINDIUM TIN OXIDE
ANTIMICROBIALMETALS (SILVER)
ANTIMICROBIALSILVER OXIDE
ANTIMICROBIALCOPPER OXIDE
UV ABSORPTION / ANTIMICROBIALTITANIUM DIOXIDE
UV ABSORPTION / ANTIMICROBIALZINC OXIDE
UV ABSORPTION / HARDNESSCERIUM OXIDE
HARDNESSSILICONE CARBIDE
HARDNESSDIAMOND
MECHANICAL STRCLAY
HARDNESSZIRCONIA
HARDNESSALUMINA
HARDNESSSILICA
COLOR / MECHANICAL STRCARBON BLACK
PROPERTYMATERIAL
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• The smaller the particle, the shorter the range of the interactiveforces between them
– The steric stabilisation barrier doesn’t need to be so thick
BUT
• The surface area per gram of particles gets bigger and bigger,so the amount of dispersant required increases
Thus, on theoretical grounds, smaller particles require
larger amounts of dispersants
WHATWHAT’’S NEEDED TO STABILISES NEEDED TO STABILISE
NANOPARTICLES?NANOPARTICLES?
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• When two particles with
absorbed polymeric or
oligomeric chains come
together, the chains are forced
to intermingle or to compress
• Generally this intermingling or
compression is energetically is a
LESS favourable state. The
particles are therefore kept
apart
• Polymeric dispersants used to
generate the steric stabilisation
layer
Localised high concentration of polymer
through compression or interpenetration gives
entropic repulsion and/or increased osmotic
pressure
STERIC STABILISATION OF PARTICLESSTERIC STABILISATION OF PARTICLES
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DISPERSANT DESIGNDISPERSANT DESIGN
Single point anchorRandom
• Pigment dispersants contain anchoring and stabilising segments
Linear comb Branched / crosslinked
comb - brush
AB block
BAB block
• For solvent based dispersants anchor groups tend to be polar / ionic.
• The stabilising segments need to be soluble in the continuous medium
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CRITERIA FOR THE STERIC STABILISINGCRITERIA FOR THE STERIC STABILISING
POLYMER CHAINSPOLYMER CHAINS
Solubility/Polymer Chain Chemistry
• The stabilisation chain must be soluble in the liquid phase.Must be a “better than theta” solvency system.
• End Use Compatibility – the chain must be compatible withresin/binder after solvent has evaporated. Otherwise film propertiessuch as haze, durability and adhesion may be degraded.
Polymer chain length
• The chain must be long enough to form a barrier of the requiredthickness
• Too long a chain tends to aid desorption
Ability to control composition and molecular weight of the steric chainsegment is critical in dispersant design
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WHAT MAKES A GOOD DISPERSANT?WHAT MAKES A GOOD DISPERSANT?
• Segmented architecture vs random.
• Intuitively expect controlled architecture to be best with
anchoring and soluble portions of dispersant well segregated.
• Limited ability of random structures to provide effective steric
stabilisation.
Random vs segmented structures
Random AB block copolymer Linear comb polymer
Anchoring and
soluble segments all
mixed together.
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MOL WT CONTROLMOL WT CONTROL
• Polymers have a distribution of molecular weights.
• Therefore even if the average mol wt of stabilisation chain is correct therewill be lot of material where the stabilisation chain is too small or too big
• The concept is the same for block or comb structures
Schematic illustration of block colplymers with broad mol
wt distribution
Schematic illustration of linear
comb with broad mol wt
distribution of steric chains
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SOLVENT HYPERDISPERSANTSSOLVENT HYPERDISPERSANTS
INFLUENCE OF SOLVENT SOLUBILITYFIRST RECOMMENDATION NOT RECOMMENDED
(HIGHLY SOLUBLE)
RECOMMENDED (SOLUBLE) INSOLUBLE
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Unsaturated Polyesters
And GelCoats
Thermosets/
Composites
Epoxies
Polyether -
Polyol Non-Phthalate
based
Phthalate
Based
Wire and Cable
And Compounds
Masterbatch and Compound
organic pigment inorganic and fillers
32000
D510SOLSPERSE
IRCOSPERSE
SOLPLUS
Acrylics
Polyester -
Polyol
Polyols
Liquid Colours
For Plastics
Thermoplastics
20000
R700
20000
K200
K500
3000
13650
K210
K500
30002153
2155
C825
C8002155
110003000
DP310
21000
DP310R700
D510
D540
D520
D530
D510
D520
Plasticiser
Dispersions
28000
ADDITIVES FOR THERMOPLASTICS AND THERMOSETSADDITIVES FOR THERMOPLASTICS AND THERMOSETS
D550
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SOLVENT-FREE COATINGSSOLVENT-FREE COATINGS
OVERVIEW OF 100% ACTIVE SOLSPERSE PRODUCTSOVERVIEW OF 100% ACTIVE SOLSPERSE PRODUCTS
PRODUCT
PHYSICAL FORM
ANCHOR GROUP TYPE
SOLUBILISING
CHAIN POLARITY
20000
Liquid
Basic
High
32000
Solid (MPT 30 0C)
Basic
Medium
28000
Liquid
Basic
Medium - Low
8000
Liquid
Basic
Medium - Low
41000
Liquid
Anionic
High
36000
Solid (MPT 30 0C)
Anionic
Medium
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DOSAGEDOSAGE
SOLSPERSE Hyperdispersants
X
X
20%
100
200
40%
PIGMENT
SURFACE
AREA
(m2/g)
% POLYMERIC SOLSPERSE REQUIRED BASED ON WEIGHT
OF PIGMENT IN MILLBASE (% AOWP)
2mg Polymeric SOLSPERSE / m2 Pigment Surface Area
This dosage can be more easily understood as % agent on weight of pigment (% AOWP)
To convert 2mg/m2 TO % AOWP use PIGMENT SURFACE AREA (BET)= % AOWP
Theoretical Amount
5
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WHICH ANCHOR GROUP IS BEST?WHICH ANCHOR GROUP IS BEST?
ACID v AMINE
on TiO2
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TYPICAL SURFACE TREATMENT ADDITIVESTYPICAL SURFACE TREATMENT ADDITIVES
PRESENT ON RUTILE TITANIUM DIOXIDEPRESENT ON RUTILE TITANIUM DIOXIDE
ORGANIC
TRIETHANOLAMINE
POLYDIMETHYLSILOXANE
TRIMETHYLOLPROPANE
SURFACTANTS
INORGANIC
ALUMINA
SILICA
ZIRCONIA
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WHAT CONTRIBUTION DOES THE SURFACEWHAT CONTRIBUTION DOES THE SURFACE
TREATMENT MAKE TO THE PROPERTIES OF TiOTREATMENT MAKE TO THE PROPERTIES OF TiO22??
KEY PROPERTYSURFACE TREATMENT
Dispersability + compatibility
in the final application
ORGANIC
Improves pigment durabilityZIRCONIA
Promotes coating durabilitySILICA
Improves pigment wetting
in the dispersion
ALUMINA
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DO PAINT PRODUCERS NEED POLYMERICDO PAINT PRODUCERS NEED POLYMERIC
DISPERSANTS TO DISPERSE TiODISPERSANTS TO DISPERSE TiO22??
Surface treatments do contribute significantly to the
dispersibility and stability of the titanium dioxide, but……………
In many cases this treatment is not enough to fulfill all
the coating requirements.
Coating properties can be enhanced further using polymeric
dispersants (gloss, haze, opacity and the ‘blueness’ of the white).
Pigment concentration in the dispersion can be increased, thus
increasing the potential for better hiding power and improved
productivity.
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CAN THE TYPE OF POLYMERIC DISPERSANT CAN THE TYPE OF POLYMERIC DISPERSANT
AFFECT THE DISPERSION PROPERTIES OF TiOAFFECT THE DISPERSION PROPERTIES OF TiO22 ? ?
The anchor group on the polymeric dispersant can influence
the extent of dispersion stability and pigment loading with
tio2
This anchor group can be acidic, neutral or basic in nature
More effective dispersants will give better deflocculation
of the tio2 resulting in higher dispersion pigment concentration,
increased gloss and reduced haze.
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POLYMERIC DISPERSANT CHOICE FORPOLYMERIC DISPERSANT CHOICE FOR
DISPERSING TiODISPERSING TiO22
SOLSPERSE 32600 - amine anchored, multiple chain,
multiple anchor type polymeric
dispersant (basic)
SOLSPERSE 36600 - acid anchored, multiple chain,
multiple anchor type polymeric
dispersant (acidic)
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GRADES OF TiOGRADES OF TiO22 AND THEIR AND THEIR
SURFACE TREATMENTS SURFACE TREATMENTS
AcidicNoSilica / Alumina TIPURE R931
AcidicNoSilica / Alumina TIOXIDE RXL
Neutral / BasicYesSilica / Alumina TIOXIDE RTC30
BasicYesZirconia / Alumina TIOXIDE TR85
BasicYesZirconia / alumina TIOXIDE TR81
BasicYesAlumina TIPURE R700
BasicYesZirconia / Alumina TIOXIDE TR92
NATUREORGANICINORGANICGRADE
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TiOTiO22 GRADE v PIGMENT CONCENTRATION : GRADE v PIGMENT CONCENTRATION :
AMINE AND ACID ANCHORED DISPERSANTSAMINE AND ACID ANCHORED DISPERSANTS
50
55
60
65
70
75
80
85
TR92 R700 TR81 TR85 RTC30 RXL R931
TiO2
Conc(%)
Dispersion System : MS Polyester
Solsperse Dosage : 2% AOWP
Dispersion Viscosity : Approx. 1 pas (1000 cps) @ low shear (37.6s-1)
32600
36600
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TiOTiO22 GRADE v GLOSS : AMINE AND ACID GRADE v GLOSS : AMINE AND ACID
ANCHORED DISPERSANTSANCHORED DISPERSANTS
55
60
65
70
75
80
85
90
95
100
TR92 R700 TR81 TR85 RTC30 RXL R931
Gloss (600)
System : MS Polyester / Melamine
32600
36600
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TiOTiO22 GRADE AND DISPERSANT CHOICE GRADE AND DISPERSANT CHOICE
Choice of optimum anchor group
can make a significant difference
- To rheology and
- Application performance
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ROUTES TO NANO PARTICLESROUTES TO NANO PARTICLES
• Top Down - Milling
• Bottom Up- Particle formation/surface treatment
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MILLING ROUTEMILLING ROUTE
• Conventional bead mills - Bead size (0.3mm +)
- Difficult to achieve <100nm
• Nano Mills - Bead size (0.05 – 0.1mm)
- Can achieve <100nm
• General rule : Particle size = Bead Size
achieved 1000
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MAGENTA UV INK JET FORMULATIONMAGENTA UV INK JET FORMULATION
100.0
72.592.0Sartomer SR 306
15.0-Solsperse 35000
12.58Ink Jet Magenta E02 VP2621
%
MILLING ROUTEMILLING ROUTE
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MILLING CONDITIONSMILLING CONDITIONS
• Bead mill with 0.3mm beads – 4 hours
- Particle size reduces from 185 ! 135nm
JN4824 Form 4Milling time vs Particle Size
100
120
140
160
180
200
0 50 100 150 200 250
Milling time (mins)
Pa
rtic
le s
ize
(n
m)
Particle size- initial (nm) Particle size- 1 day (nm)
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MILLING CONDITIONSMILLING CONDITIONS
• Bead mill with 0.1mm beads – 50 mins
- Particle size reduces from 185 ! 82nm
Ink Jet Magenta E 02 VP 2621
With
Solsperse 35000
0
20
40
60
80
100
120
140
160
180
200
0 20 30 50
Milling Time
Part
icle
Siz
e (
nm
)
Particle Size - Diameter (nm)
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MILLING CONDITIONS - SUMMARYMILLING CONDITIONS - SUMMARY
• Nano mills - Are critical for <100nm
- Particularly small beads
• As particle size reduces, surface area increases
• Dosage should be optimised for each specific PS produced
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PARTICLE FORMATION PARTICLE FORMATION –– BOTTOM UP PROCESS BOTTOM UP PROCESS
- Flame Pyrolysis
- Sol Gel
- Organic Pigmentation Processes
- Variety of Other Routes
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HOW CAN DISPERSANTS HELP?
• Dispersants may control the growth of particles, giving
smaller particles
• Dispersants may increase the solids loading achievable
before gelation. This should then give reduced shrinkage
on drying / firing, and better final product properties
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SURFACE TREATMENTSURFACE TREATMENT
WITH ADDITIVESWITH ADDITIVES
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SOLSPERSESOLSPERSE!! HYPERDISPERSANTS HYPERDISPERSANTS
Applications in Pigment/Particle Treatment
Solsperse hyperdispersants can be utilised in the manufacture of pigments
to provide a surface treatment which can improve the pigment
The anchor group of the hyperdispersant strongly adsorbs on to the pigment
surface, whilst the polymeric chain provides a high degree of steric stabilisation
Anchor GroupPolymeric Chain
Process Stage
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QUALITY PRODUCTIVITY
SOLSPERSESOLSPERSE!! FOR PIGMENT / PARTICLE FOR PIGMENT / PARTICLE
Flow Throughput/Cycle Time
Strength Decreased mechanical wear
Dispersibility Increased solids (slurry, paste)
Product Stability Improved dry pigment for milling
Treatment - Benefits
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SOLSPERSESOLSPERSE!! FOR PIGMENT FOR PIGMENT
Treatment - Quality
Quality
(strength or
brightness or
dispersibility,
etc)
Untreated
Pigment
Untreated
Pigment
+Solsperse! in
the formulationPigment
treated withSolsperse!
Solsperse!
treated pigment
+Solsperse! in
the formulation
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SOLSPERSESOLSPERSE!! GRADES FOR GRADES FOR
Surface Treatment
• Choice by solvent / medium
• By particle surface
• Dosage by surface area
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POSSIBLE PIGMENT TREATMENT OPTIONSPOSSIBLE PIGMENT TREATMENT OPTIONS
WITH SOLSPERSEWITH SOLSPERSE!! ADDITIVES ADDITIVES
STEPS TO CONSIDER WHEN INVESTIGATING USE OFSOLSPERSE! IN PIGMENT TREATMENT
• WHICH PIGMENT AND WHICH SYNTHETIC ROUTE?
• Organic or inorganic?
• WHICH APPLICATION IS THE PIGMENT DESIGNED FOR?
• Ink or paint?
• CHOOSE THE BEST SOLSPERSE! AGENT FOR PIGMENT SURFACE AND DESIRED
APPLICATION
•CONSIDER BEST APPROACH TO GETTING AGENT ONTO PIGMENT SURFACE, ie WHERE TO ADD SOLSPERSE!?
• Add during particle formation e.g. azo precipitation after coupling
• To an aqueous phase/as an emulsion prior to drying or milling (ensure homogeneous)
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APPLICATIONS IN PIGMENT TREATMENTAPPLICATIONS IN PIGMENT TREATMENT
DOSAGE
Generally much less agent is utilised compared
with conventional solsperse applications
But for NANO:-
For inorganic pigments around 5-10% active SOLSPERSE!
agent should be used
For organic pigments around 20-40% active SOLSPERSE!
agent should be used
(THESE LEVELS ARE BASED ON NON DRYING PROCESSES)
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APPLICATIONS IN PIGMENT TREATMENTAPPLICATIONS IN PIGMENT TREATMENT
Pigment Type
Potential Points of Addition (very dependent on pigment producer)
Benefits Seen (where known)
Mono Azo Reds
Rubines (Red 57.1)
• Add as an emulsion with rosin solution • Can be added after laking stage, but ... • Best results obtained if Solsperse/rosin
solution added to coupling stage
Inks: Better gloss, intensity Higher transparency Better strength development Reduced cycle times of production Improved dispersibility and reduced viscosity Improved performance in packaging gravure inks
Red Lake C (Red 53.1) Lithol Reds (Red 49.1) Permanent Red 2B (Red 48s)
• Best results seen when added as an emulsion
after coupling but prior to laking
Transparent, easy to disperse pigments for offset paste inks or gravure liquid inks
Diarylide Yellows
Yellow 12, Yellow 13
• Added as a solution (in acetic acid) during the
coupling stage • Can be used also as an alternative to post-
treatment with rosins or fatty amines • Can be added as an emulsion prior to drying
Stronger, brighter pigments Improved dispersibility in inks Improved dispersibility Control opacity/transparency
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APPLICATIONS IN PIGMENT TREATMENTAPPLICATIONS IN PIGMENT TREATMENT
Benefits Seen
(where known)
• Added during or after milling processes • Or added during solvent crystallisation • Or added as an emulsion prior to drying
Improved rheology in solventborne paint and ink systems Increased colour strength
Pigment TypePotential Points of Addition(very dependent on pigment producer)
Phthalocyanine Blues Blue 15.4, 15.3
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Pigment Type
Potential Points of Addition (Very dependent on pigment producer)
Benefits Seen (Where known)
Inorganics
Synthetic iron-oxides - Yellow 42 - Red 101
• Post treatments after high temperature processing
• Improved dispersibility in solvent paint system
• Higher strength pigment in solvent borne paint formulation
APPLICATIONS IN PIGMENT TREATMENTAPPLICATIONS IN PIGMENT TREATMENT
Titanium Dioxide
• Added as an emulsion prior to drying
•
• Increased solids loading in the slurry
• Improved performance in plastics final application
• Improved performance in solvent systems
Zinc Oxide
• Dependent on pigment manufacturer
• Improved application performance
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APPLICATIONS IN PIGMENT TREATMENTAPPLICATIONS IN PIGMENT TREATMENT
Pigment Type
Potential Points of Addition (Very dependent on pigment producer)
Benefits Seen (Where known)
Iron blue or Milori blue - Blue 27
• Added to presscake prior to drying
• As above
• Improved dry pigments for publication gravure applications - improved dispersibility
• Decreased mechanical abrasion
Fillers (ATH, talc, kaolin, CaCO3 etc)
• Added to an aqueous slurry as emulsion prior to drying
• Improved application performance in plastics
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SOLSPERSESOLSPERSE!! HYPERDISPERSANTS HYPERDISPERSANTS
APPLICATIONS IN PIGMENT TREATMENT
EMULSION/SOLUTION PREPARATIONSOLSPERSE! 3000 EMULSIONS
NON-IONIC EMULSION
1. MELT & MIX TOGETHER 20 PARTS SOLSPERSE! 3000 AND 5 PARTS SYNPERONIC A14 SYNPERONIC A14: C13-C15 MIXED ALCOHOL + 14 ETHYLENE OXIDE UNITS
2. WITH HIGH SHEAR STIRRING POUR MIXTURE INTO 75 PARTS OF WATER WHICH IS AT 50°C
ANIONIC EMULSION
1. MELT 25 PARTS SOLSPERSE! 3000 AND POUR INTO A SOLUTION OF 2.5 PARTS
TRIETHANOLAMINE/72.5 PARTS WATER WHICH IS AT 50°C AND BEING STIRRED RAPIDLY
USING A HIGH SHEAR MIXER THESE EMULSIONS ARE STABLE FOR SEVERAL MONTHS AT AMBIENT TEMP. & IN pH2-pH10
SOLSPERSE! 3000 SOLUTION
SOLSPERSE! 3000 12.5
BUTYL CELLOSOLVE 12.5
1N KOH SOLUTION 75.0
SLURRY THE SOLSPERSE! P850 IN THE KOH SOLUTION AND CLARIFY THE SLURRY BY THE ADDITION OF THE BUTYL CELLOSOLVE
FINAL SOLUTION IS SLIGHTLY HAZY AND AFTER STANDING 4 DAYS A SMALL AMOUNT OF PRECIPITATE
SETTLES WHICH IS READILY RE-DISPERSED ON STIRRING
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TECHNICAL SERVICE / DEVELOPMENTTECHNICAL SERVICE / DEVELOPMENT
CAPABILITYCAPABILITY
• Bead Mills - Conventional Range (x3)
- Nano Mill Shortly
• Standard Additive recommendation based on enquiry
• Development capability for Polyester, Acrylics, PU,
Dispersants
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DISPERSANT RECOMMENDATIONS FORDISPERSANT RECOMMENDATIONS FOR
NANOPARTICLE APPLICATIONSNANOPARTICLE APPLICATIONS
SOLSPERSE 36000
or
SOLSPERSE 39000
SOLSPERSE 3000
or
SOLSPERSE
11000/11200
[SOLSPERSE 27000/54000
if very hydrophobic]
Larger
Nanoparicles
SOLPLUS D520
or
SOLPLUS D510
SOLSPERSE 21000
or
SOLSPERSE 8000
SOLPLUS D540
or
SOLSPERSE 20000
Smaller
Nanoparticles
Medium polarity
Solvents
e.g. esters, ketones,
Aromatics, glycol,
esters, terpineol
Low polarity
solvents
e.g. aliphatics
Alcohol / water based
Sol-gel process
Note: A few products contain phosphorus, and this may cause
problems in some advanced electronic applications
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PLEASE CONTACT US FOR YOUR
DISPERSANT NEEDS
QUESTIONS ?
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