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Rheovis® AT 120

Rheology Modifier of Liquid Detergent

Care Chemicals and Formulation


April, 14, 2011

22/07/2010 1
Rheovis® AT 120
ƒ copolymer based on:
methacrylic acid and acrylic acid esters
ƒ associative thickener
ƒ hydrophobic modified alkaline soluble
emulsion (HASE)
ƒ concentration: ca. 30%
ƒ pH value: ca. 3
ƒ milky, low viscous dispersion
ƒ viscosity: ca. 30 mPas
Brookfield RVT SP 1 @ 100 rpm, 23°C
ƒ density: ca. 1.05 g/cm3 @ 23°C

22/07/2010 2
Facts
Polyacrylate Rheology Modifier
Rheovis® AT 120

¾ alkaline soluble
=> thickening effect in the alkaline pH range: pH > 7
¾ HASE-type = hydrophobic modified alkaline soluble emulsion
(associative thickener)
¾ due to association with hydrophobic formulation components
formation of network structure possible, which can increase the
thickening effect
¾ shear thinning rheology, realization of a yield point possible
¾ as ionic polymer sensitive toward high salt content,
but improved tolerance compared to non-associative thickeners
of ASE-type = alkaline soluble emulsion

22/07/2010 3
Rheovis® AT 120
basic properties
alkaline soluble: pH-dependence

η = f(pH)
@ 1wt% active Rheovis® AT 120
Brookfield SP 62 @20 rpm, 20°C

10000
viscosity in mPas

1000 dissolved =>

100

10
<= undissolved

1
6 7 8 9 10 11 12 13
pH
22/07/2010 4
Rheovis® AT 120
basic properties
alkaline soluble: concentration dependence

η = f(concentration)
@ pH 8.5

10000
Brookfield SP 62 @20 rpm, 20°C
viscosity in mPas

1000

100

10

1
0,25 0,75 1,25 1,75 2,25 2,75
wt% rheology modifier (active)
22/07/2010 5
Rheovis® AT 120
basic properties
alkaline soluble: influence of salt/electrolyte (NaCl)

η = f(NaCl concentration)
@ 1wt% active Rheovis thickener
pH 8.5
Brookfield SP 62 @20 rpm, 20°C

10000
viscosity in mPas

1000

100

10

1
0,0 0,2 0,4 0,6 0,8 1,0 1,2
NaCl-concentration in %
22/07/2010 6
Rheovis® AT 120
basic properties
shear thinning behaviour
η = f(shear rate)
@ 1wt% active Rheovis® AT 120, pH 8.5, 23°C
viscosity / Pa·s RVM - cylinder-system CC27
2
10
Vup and
531/39
down
1
10

0
10

-1
10

-2
10 -2 -1 0 1 2 3
10 10 10 10 10 10
-1
22/07/2010 shear rate / s (by Physika MCR 301)
n: / Auftraege / 92622 / 92622_00.opj - [ Graph 1 ]
7
Rheology Modifier Tests
liquid detergents
test procedure: post addition

post addition

22/07/2010 8
Formulation Examples

raw materials in wt% active

Formulation 2495/03
Lutensit® A-LBS 17.9
Lutensol® A 7N 20.0
coconut fatty acid 8.5
(Edenor K8-18)

KOH 5.0
sodium citrate x 2 H2O 3.0
1,2-propylene glycol 8.0
ethanol 2.0
water add to 100.0
WAS 46.4
Washing Active Substance = wt% (Lutensit A-LBS + nonionic surfactant + fatty acid)
22/07/2010 9
viscosity in mPas
Brookfield SP 62 @20 rpm, 20°C

22/07/2010
po no
ly th

1000
1200
1400

200
400
600
800

0
ol ic
fa ke
tty ne
ac r
id
es
te
r
al
gi
na
te

A
SE
H
A
SE
3
Viscosity

H
A
SE
2
H
R A
he SE
ov 1
is
®
Formulation Examples

A
T
12
0

Transmission in %
@440 nm, RT
po no
with 1.5 wt% active rheology modifier

ly th
100
120

20
40
60
80

ol ic 0
fa ke
tty ne
post addition into formulation F 2495/03

ac r
id
es
te
r
al
gi
na
te

A
SE
H
A
SE
3
H
A
SE
2
Transparency

R H
he A
SE
ov
is 1
®
A
T
12
0
10
Formulation Examples

raw materials in wt% active

Formulation 2495/07
Lutensit® A-LBS 13.4
Lutensol® A 7N 10.0
coconut fatty acid 8.5
(Edenor K8-18)

KOH 4.4
sodium citrate x 2 H2O 3.0
1,2-propylene glycol 8.0
ethanol 2.0
water add to 100.0
WAS 31.9
Washing Active Substance = wt% (Lutensit A-LBS + nonionic surfactant + fatty acid)
22/07/2010 11
viscosity in mPas
Brookfield SP 62 @20 rpm, 20°C

22/07/2010
po no
ly th

1000
1200
1400
1600
1800

200
400
600
800

0
ol ic
fa ke
tty ne
ac r
id
es
te
r
al
gi
na
te

A
SE
H
A
SE
3
Viscosity

H
A
SE
2
H
R A
he SE
ov 1
is
®
Formulation Examples

A
T
12
0

Transmission in %
@440 nm, RT
po no
with 1.5 wt% active rheology modifier

ly th
100
120

20
40
60
80

ol ic 0
fa ke
tty ne
post addition into formulation F 2495/07

ac r
id
es
te
r
al
gi
na
te

A
SE
H
A
SE
3
H
A
SE
2
Transparency

R H
he A
SE
ov
is 1
®
A
T
12
0
12
Rheovis® AT 120

¾ product form: low viscosity dispersion


=> easy and exact to dose
¾ fast dissolution in alkaline solutions
¾ product can be added as is,
e.g. within the blending process or as post addition
¾ no pre-dissolution or heating necessary
¾ no preservation of the product necessary due to acidic pH
¾ low odour
¾ good price/performance ratio
¾ perfect rheology modifier for liquid detergents

22/07/2010 13
Rheology Modifier
— RHEOVIS® FRC

BASF Asia Technical Center


Care Chemicals and Formulators

22/07/2010 14
Introducing RHEOVIS® FRC

RHEOVIS® FRC is a new multi-


functional, cationic liquid dispersion
polymer (LDP) for application in
aqueous-based fabric care and
household products:

RHEOLOGY MODIFIER

STABILIZER

PRODUCTION AID
22/07/2010 15
Benefits of Using RHEOVIS® FRC in Fabric
Rinse Conditioners

„ Effectively thickens fabric softener actives


- Degree of thickening depends on the type and concentration
„ Imparts dispersion stability to dilute fabric softeners to
help
- Provide long-term stability to ester quats
- Improve stability of fragrance emulsion in the fabric softener
- Stabilize viscosity
„ Non-associative thickening for
- Enhanced shear tolerance compared to associative rheology
modifier

22/07/2010 16
Physical/Chemical Properties of RHEOVIS® FRC

Appearance White dispersion


Chemical
Cationic, acrylic-based homopolymer
Description
Liquid dispersion polymer (biodegradable ester
Product Form
continuous phase)
pH (as is) 3.5
Shelf Life 1 year
Aqueous solution of RHEOVIS® FRC is a non-
Rheology Newtonian fluid that is shear-thinning with little
to no thixotropy

Incorporation 0.1 – 5%, based on the weight of the finished


levels product

22/07/2010 17
Viscosity Build of Fabric Rinse Conditioners

0.1% RHEOVIS FRC 0.4% RHEOVIS FRC

1400
Viscosity (mPa.s) 60

1200
rpm, Spindle #2
LV Brookfield

1000
800
600
400
200
0
STEPANTEX VK-90 Armosoft DEQ
7% active Ester Quat*
Viscosity build is dependent on type of quaternary fabric
softener active and level of rheology modifier
* Armosoft® is a registered trademark of AkzoNobel and
STEPANTEX® is a registered trademark of Stepan Company
22/07/2010 18
Viscosity as a Function of Ester Quat Concentration

0.1% RHEOVIS FRC 0.4% RHEOVIS FRC


1400
(mPa.s) 60 rpm, Spindle #2
LV Brookfield Viscosity

1200
1000
800
600
400
200
0
3 5 6 7
Armosoft DEQ (% )
Effective viscosity build with RHEOVIS® FRC
at low incorporation levels
22/07/2010 19
Stabilization of Dilute Fabric Rinse Conditioners

„ Fabric rinse conditioners are a dispersion of quaternary (quat)


ammonium compounds in water
z Typically, ester-based quats are used due to biodegradability
advantages
„ Dispersion stability depends on
z Viscosity and activity of the formulation
„ Dilute fabric softeners often exhibit
- Poor stability of the dispersion
- Sensitivity to high shear

22/07/2010 20
RHEOVIS® FRC:
Added to Dilute Rinse Conditioners

Ingredient Addition (%) LV Brookfield Viscosity


(mPa.s) 60 rpm, Spindle 2
Water 96.6 <100
Armosoft® DEQ 3.3 76
RHEOVIS® FRC 0.1 186

Water 96.5 <100


Armosoft® DEQ 3.3 76
RHEOVIS® FRC 0.2 248

Efficient viscosity build with RHEOVIS® FRC


22/07/2010 21
Test Condition

„ Rewoquat WE 18 (Degussa) , TE 90 (Tianjing Xian’guang)


„ Original viscosity
„ Viscosity with Rheovis FRC
„ Stability at -5C (24 hours) and 40C (24 hours)

22/07/2010 22
Result (2-1)

Original add 0.1%


0.2% FRC 0.3% FRC
Viscosit fragrance
mPa.S y (20C,S2,60r (23C,S2,60rpm) (23C,S2, -5C 40C
pm) 60rpm)
(Brookfield) (24C,S2, (23C,S3, (23C,S3,
60rpm) 60rpm) 60rpm)

4%
TE 90 25 85 212 450.9 473.9 355
(Commercial)

22/07/2010 23
Result (2-2)

add 0.1%
Original 0.2% FRC
fragrance
mPa.S Viscosity
(23C,S2,60 -5C 40C
(20C,S2,60rpm)
(Brookfield) (23C,S2,60 rpm)
rpm) (23C,S3,60 (23C,S3,60
rpm) rpm)
5%
WE 18 157 214 412 400 403.9
(Commercial)

22/07/2010 24
RHEOVIS® FRC
Increases Yield Point of Dilute Rinse Conditioners

The yield point is defined as the minimum


required force to initiate flow, and may also
represent the ability of a formulation to maintain
solid particles in suspension
- Typically for fabric rinse conditioners, the
higher the yield point, the higher is the
suspension property of the dispersion

22/07/2010 25
Rheology Versus Storage Stability

RHEOVIS® FRC Preparation Time Sweep Yield Point Flow Curve** 3-Month Storage
Amount (%) Stability at 40 oC
(Pa)*

Dilute Softener Base (3% actives)

0 Low Shear Stable <0.01 Control Fail

0 High Shear Unstable <0.01 NA Fail

Dilute Softener Base (3% actives) + RHEOVIS® FRC

0.1 Low Shear Stable 0.08 Improved Pass

0.1 High Shear Stable 0.09 Improved Pass

0.2 Low Shear Stable 0.32 Improved Pass

0.2 High Shear Stable 0.25 Improved Pass

* Oscillation Sweep
** Suspension properties compared to Control from flow curve

Use of RHEOVIS® FRC in dilute fabric softeners imparts


excellent stabilization to fabric softeners, whether prepared
under high or low shear
22/07/2010 26
Impact of Fragrance on Formulation Stability

Ingredient Addition (%) Addition (%) Addition (%)

Water 96.5 96.5 96.5


STEPANTEX® VK-90 3.3 3.3 3.3
RHEOVIS® FRC - 0.1 0.4
Fragrance 0.2 0.2 0.2

LV Brookfield Viscosity (mPa.s),


30 rpm, Spindle 2
-- 13 129
Stability Separates Yes Yes
Appearance Oil/particulates Slight Creamy
particulates

RHEOVIS® FRC stabilizes the fragrance


emulsion in the dilute fabric rinse conditioner
22/07/2010 27
Long-term Stability of Fabric Rinse
Conditioners

„ Fabric rinse conditioners based on ester quat typically


suffer from hydrolysis of the quat to fatty acid and amine
z Over time the fatty acid builds up and causes the
product to thicken and eventually to solidify
z Higher temperatures increase hydrolysis rate

Thus, storage and transportation conditions will affect long-


term stability

22/07/2010 28
RHEOVIS® FRC – Shelf Life

„ RHEOVIS® FRC was compared to typical LDP products


„ Evaluated for product separation/settling at room temperature and
at 45oC for 12 weeks
No sedimentation
observed for
RHEOVIS® FRC
25
Sedimentation (%)

20
15
10 Typical LDP
5 RHEOVIS FRC
0
25 45
Temperature (oC)
New LDP technology yields extended shelf life for RHEOVIS® FRC
22/07/2010 29
Summaries - RHEOVIS® FRC

„ Fabric Rinse Conditioner Efficacy Studies


z Effectively thickens fabric softener actives
z Imparts stability to dilute fabric rinse conditioners
z Helps to stabilize the fragrance emulsion in fabric rinse
conditioners
z Aids in post production viscosity adjustments and improves stability
of ultra fabric rinse conditioners
z Non-associative thickening that enhances shear tolerance

22/07/2010 30

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