TDS-103 Dispersion Techniques Carbopol Polymers PDF

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TECHNICAL DATA SHEET

TDS-103
Edition: October 15, 2007
Previous Edition: January, 2002

Dispersion Techniques for Carbopol®* Polymers


Carbopol® polymers are highly water and polar most appropriate. Extremely high-shear mixers
solvent soluble polymers which function as efficient such as Waring blenders or rotor-stator
thickeners and stabilizers for suspensions or homogenizers should be avoided or carefully
emulsions. Much of the exceptional utility of the employed. The mixing intensity generated by this
Carbopol® polymers results from the hydrophilic type of mixer can shear the opened (hydrated)
nature of the polymer. A single particle of polymers resulting in permanent viscosity loss. In
Carbopol® polymer will wet out very rapidly when some cases, this loss can be as high as 50%.
put into water. Like many fine particulate powders, Conventional impellers, such as propellers
Carbopol® polymers tend to clump when improperly or turbines do not impart excessively high shear
added to the solvent. rates. They can be used to mix mucilages for
The surface of a powder aggregate solvates to form extended periods with virtually no decrease in
a tough outer layer which prevents complete polymer efficiency.
wetting of the interior polymer particles. This If in-line mixers such as colloid mills or
results in dispersion defects such as grainy texture, homogenizers are used, the Carbopol® polymer
reduced viscosity or the presence of insoluble should be initially wetted-out with moderate rate
particles resembling fish eyes. agitation. Therefore, the mixing time using the high
To prepare high quality and reproducible shear mixers will be minimized. If a homogenizer is
dispersions of Carbopol® polymers, the proper employed, strive to use the lowest shear rate and
dispersing technique must be carefully followed. the shortest mixing time to achieve a homogeneous
mixture.
I. Direct Addition of Carbopol® Polymers When mixing, submerge the impeller until it is very
into Water close to the bottom of the vessel and angle the
The proper method to use when adding Carbopol® mixer to generate a vortex which is one to one-and-
directly to water depends on the quantity and one half impeller diameters. Slowly sift the polymer
concentration of the dispersion to be prepared. into the vortex of the agitating liquid (approximately
A. Small Quantity Batch Dispersions 1200 rpm). Continue the agitation for about 20
minutes or until a lump-free dispersion is attained.
Dispersions of several hundred milliliters to several In some cases when a Lightnin' Mixer is employed,
gallons with concentrations of up to 1.5 weight two impellers on a common shaft are
percent Carbopol® polymer can be practically recommended. The top impeller rapidly disperses
prepared by sifting the dry polymer into rapidly the polymer before the undesirable, partially-
agitating water. hydrated lumps are formed. A sifting device such
Aqueous surface wetting and dispersion of as a coarse sieve or a non-corrosive 20-mesh
Carbopol® polymer is best achieved with moderate metallic screen should be used to slowly sprinkle
rate agitation of approximately 800-1200 rpm. the Carbopol® polymer into the vortex of the water
Motorized mixers such as the Eppenbach, generated by the mixer. The sifting method allows
Colframo, Arde-Barinco, Janke and Kunkel or the slow, controlled addition of the dry Carbopol®
Lightnin' Mixer with a conventional open-blade polymer, enabling each particle to wet out on the
impeller (pitched marine or saw tooth propeller) are water vortex. The sieve or screen permits the

Lubrizol Advanced Materials, Inc. / 9911 Brecksville Road, Cleveland, Ohio 44141-3247 / TEL: 800.379.5389 or 216.447.5000
The information contained herein is believed to be equipment used commercially in processing these Materials, Inc.’s direct control. THE SELLER MAKES NO
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suitability for particular applications or the results to be disclosed. Full-scale testing and end product OF MERCHANTABILITY AND FITNESS FOR A
obtained therefrom. The information is based on performance are the responsibility of the user. Lubrizol PARTICULAR PURPOSE. Nothing contained herein is
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not necessarily indicate end product performance. customer assumes all risk and liability of any use of as an inducement to practice any patented invention
Because of the variations in methods, conditions and handling of any material beyond Lubrizol Advanced without permission of the patent owner.
For further information, please visit www.pharma.lubrizol.com
Lubrizol Advanced Materials, Inc. is a wholly owned subsidiary of The Lubrizol Corporation
* Trademark owned by The Lubrizol Corporation
© Copyright 2007 / The Lubrizol Corporation
2

break-up of any loose polymer or agglomerates due


to the static charge on the particles. A metallic Selecting Neutralizers for
screen decreases the tendency to build more static High Alcohol Solutions
charge on the particles as they are sifted. • Metallic alkali (NaOH, KOH, etc.) will
Once all the dry polymer has been introduced, neutralize Carbopol® polymers with less
continue agitating at the moderate to rapid rate for than 20% ethanol.
10-15 minutes. Reduce the speed to avoid the • Triethanolamine (TEA) will neutralize
entrapment of excess air. Carbopol® polymers up to 50% ethanol
For emulsions, add oils and emulsifiers to form the solution.
emulsion prior to neutralizing the Carbopol® to build • 2-Hydroxypropyl ethylene diamine
emulsion viscosity. Neutralization of Carbopol® is (Quadrol®) will neutralize Carbopol®
accomplished with a suitable alkali or amine base. polymers up to 70% ethanol solution.
For the order of neutralizer addition in gel products,
see the Carbopol® Troubleshooting Guide.
B. Large Quantity Batch Dispersions
Dispersion volumes ranging from tens of gallons to
hundreds of gallons at concentrations of Carbopol®
polymers of up to three weight percent may be
prepared with an eductor or flocculant disperser.
This technique is a fast, inexpensive means of
dispersing Carbopol® polymers with reduced
dusting.
Figure 1 shows how the rate of dispersion
increases with an increase in water pressure.
Figure 2 shows the basic design of the eductor. It
is a small, inexpensive, metal or plastic, non-
moving plumbing valve which exerts a partial
vacuum on the powder inlet via the Bernoulli effect.
Carbopol® polymer is pulled from the eductor funnel
1. Cowles Blade—Not recommended due to high shear. into the eductor valve throat. The partial vacuum is
2. Paddle Blade—Frequently used when blending operations follow created by the flow of incoming make-up water
initial dispersion of Carbopol polymer. through the venturi of the eductor throat. Water
®
3. 3-Blade Marine Impeller—Excellent choice for dispersing Carbopol turbulence within the valve wets out the polymer to
polymer. Impeller of choice when making emulsions.
enable the formation of quality dispersions.
4. Foddler Impeller—Poor mixing due to low shear.
5. Hi-Lift Impeller—High shear: use with caution. The eductor outlet should have enough piping (4-5
ft.) to build sufficient back pressure to direct the
polymer/ water slurry into an agitated mix tank filled
with water to complete polymer hydration.
Note: Dispersions of Carbopol® polymers made
to a precise solids level for analytical viscosity Eductors can disperse 22.7 kg (50 lb>) of polymer
testing should follow Lubrizol Standard Testing in five to ten minutes with up to 3.0% polymer
Procedure 430-I, "Brookfield Viscosity (low concentration. Determining the exact eductor and
shear)." size required for the specific application can best
be determined from the technical bulletins and
advice of an eductor manufacturer.
Note: Select an eductor which is capable of a
solid particle dispersion. Do not use a liquid
eductor model. The funnel may be replaced by
a flexible hose with stainless steel end tube to
enable direct vacuum pick-up from the box of
Carbopol® polymer.
3

Figure 1 Further information regarding eductors can be


Dispersion Rate of Carbopol® Polymers with an Eductor obtained from these manufacturers:
PENBERTHY
P.O. Box 112
Feed Rate of Carbopol Resins lb/min

26 Prophetstown, IL 61277
Phone: (815) 537-2311
22
FAX: (815) 537-5764
18 AMETECK INCORPORATED
Poor dispersing Division of Schutte and Koerting
14 below 5 gal/min
or 35 psig
2233 State Road
Recommended Bensalem, PA 19020
10 Phone: (215) 639-0900
Operating Area
FAX: (215) 639-1597
6
FOX VALVE DEVELOPMENT
2 CORPORATION
Hamilton Business Park, Unit 6A
2 6 10 14 18 22 26 30 Franklin Road
Dover, NJ 07801
Water Flow Through Eductor, gal/min Phone: (201) 328-1011
FAX: (201) 328-3651
DICKENS & WILLIAMSON
Figure 2 INCORPORATED
Eductor P.O. Box 25009
Charlotte, NC 28212
Phone: (704) 537-0304
FAX: (704) 245-1977

C. Large Quantity Continuous Production


Dispersions
The production of good quality, high-solids
Carbopol® polymer dispersions from a continuous
production scheme is possible with a mechanical
in-line powder disperser. Mechanical dispersers
use the principle of a high velocity eductor coupled
with the mechanical working configuration of an in-
Funnel line homogenizer to rapidly disperse and wet each
individual polymer particle instantaneously. This
highly turbulent, high-shear mixer operates at such
a rapid rate that the particles are wetted and
expelled prior to polymer swelling. Lump formation
Air vent holes
and polymer degradation from mechanical shearing
are eliminated.
The valved powder hopper feed of the mechanical
disperser can significantly reduce the level of air
entrapment or foaming. Dispersed particles are
expelled from the disperser directly in a tank
with low/moderate agitation. Table 1 provides
Eductor outlet comparative outline of mechanical dispersers
Make-up
water in and their features.
4

Further information regarding mechanical disper-


sers can be obtained from the following Tips for Using an Eductor
manufacturers or distributors.
YTRON®
• Avoid using hot water. The water vapor
will prematurely swell the polymer end clog
Dr. Karg GmbH
the eductor.
Osternacherstrasse 50
D-8210 Prien am Chiemsee • A minimum 3/4-inch (2 cm) diameter pipe
Germany end 35 psig (1.2 atm) water pressure is
Phone: 08051/1457 required for an eductor. Constant pressure
must be maintained. If necessary, include
QUADRO™ PROCESS INC. a pump for inlet water.
72 King Street South
St. Jacobs, ON
• The eductor should be installed with easily
removable plumbing fittings to facilitate
Canada NOB 2N0
cleaning. The discharge must be located
Phone: (519) 664-3724
above the liquid level of the tank to prevent
SILVERSON MACHINES LTD. back pressure.
Waterside Chesham, Bucks • Prevent plugging of the eductor throat by
HP5 1 PQ, England starting with a clean eductor and initiating
United Kingdom the water flow before adding the
Phone: 0494786331 preweighed polymer to the eductor funnel.
NORTH AMERICAN If the eductor does plug with dry polymer,
SILVERSON MACHINES LTD. care should be taken when cleaning so that
P.O. Box 589 the eductor orifice size is not altered.
50 Industrial Drive • Tapping the funnel manually or with an
East Longmeadow, MA 01028 inexpensive vibrator will prevent Carbopol®
Phone: (413) 525-4825 polymer from sticking to the funnel.
ARDE BARINCO INC.
500 Walnut Street
Norwood, NJ 07648
Phone: (201) 784-9880 A handy technique to break the foam is to partially
collapse the polymer by the addition of a very low
D. Carbopol® Polymers and Foam level of strong mineral acid. The yield value is
Some foaming can occur in the preparation of reduced and the trapped air surfaces. Phosphoric
Carbopol® polymer in water dispersions, particularly or hydrochloric acid is effective at O.5% on the
with Carbopol® 1342 and 1382. The significant weight of Carbopol® polymer. A 1.0 weight percent
yield value of these dispersions (even as dispersion of Carbopol® polymer would require
unneutralized polymers) can result in the formation 0.005 weight percent or 50 ppm H3PO4 or HC1.
of a persistent foam. This level of acid results in no significant
contribution of salt when neutralizing Carbopol®
polymer. Therefore, the viscosity of the end
Table 1 product is unaffected. Organic acids such as citric
Mechanical Dispersers for Carbopol® Polymers or lactic acid are not recommended because they
Maximum are weaker acids and would yield higher
Carbopol Water
Manufacturer/ Carbopol
Model Polymer Polymer Flow Rate concentrations of residual salts upon neutralization.
Distributor Capacity Solids (lbs./hr.)
(lbs./hr.)
(wt. %)
YTRON
ZC 1200 15* 15,000
QUADRO
Silverson
Silverson
Machines Ltd., 7500 15-20* 50,000
Flashblend
UK
Arde Vaccuum
Arde Barinco Inc. 1000 4 30,000
Dilumelt
* Dispersions of greater than 5 weight percent Carbopol® polymer become
dense, solid-like, and impractical to pump or handle.
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II. Indirect Addition of Carbopol® Polymers C. Dispersing Carbopol® Polymer in Polar


into Water Organic Systems
Since polar organic solvents prevent the rapid
In emulsions and alcoholic/water gels, optimum swelling of Carbopol® polymers, sifting the
dispersions can best be prepared using the indirect polymers may be optional. In pure solvent or at
method of adding Carbopol® polymer to a high concentrations in water, the Carbopol®
formulation. The dispersion preparation can be polymer can be directly added with minimal
simplified by blending Carbopol® polymer and a agitation. When using pure solvent, add the
liquid nonsolvent, such as the oil phase of an polymer/solvent slurry to water, or vice versa, with
emulsion, ethanol/isopropanol, or a hydrophobic vigorous (800-1200 rpm) mixing. Polar organic
surfactant, to form a premix. Any non-solvent of solvents include alcohols and glycols.
Carbopol® polymer which is part of the product's
formulation or is an acceptable additive to the D. Dry Blending of Carbopol® Polymers
product may be used. A solid concentration of up To reduce addition and mixing time, Carbopol®
to 10 weight percent of Carbopol® polymer can polymers can be initially dry blended with other dry
work. ingredients. The blend is usually free-flowing and
A. Oil-in-Water Emulsions free of lumps if the polymer constitutes less than
half of the total dry weight. Avoid blending
Combine the ingredients of the oil phase and, Carbopol® polymer with polyvinylpyrrolidone (PVP),
if required, heat until all materials are liquid. cellulosic polymers or other gums and clays.
Temperature must not exceed 60°C. Add These blends may give water insoluble complexes
Carbopol® polymer to the oil phase with moderate or may prevent proper swelling of Carbopol®
to vigorous agitation of 600-800 rpm. Immediately polymer.
follow with the addition of water containing the
appropriate inorganic or amine base to neutralize Note: Test the compatibility of Carbopol®
and thicken the Carbopol® polymer and set the polymer in the oil in which it is to be dispersed.
emulsion. Increase the rate of agitation to 1000- In the presence of some polar oils (aromatic or
1200 rpm and mix for 15-20 minutes or until a dicarboxylic acid esters) or molten oils above
smooth, non-grainy texture is apparent. 60°C, Carbopol® polymer will physically
plasticize, hindering stable emulsion formation.
B. Aqueous Suspension from Insoluble Dispersing Carbopol® polymer directly into the
Concentrates of Carbopol® Polymers water in these cases will result in smooth,
Non-solvent dispersions with Carbopol® polymer in stable emulsions.
mineral oil, mineral spirits, kerosene and low HLB
non-ionic surfactants can be prepared using
moderate agitation to wet out the polymer prior to
its addition into water. This bulk dispersion of the
polymer by a non-solvent delays the rate at which
the Carbopol® polymer swells or hydrates into
water, thus minimizing clumping or the formation of
inferior quality aqueous dispersions.
These non-solvent dispersions of Carbopol®
polymers should be used immediately to avoid solid
polymer settling or agglomeration of the polymer
due to plasticization.

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