J. Coat. Technol. Res.

https://doi.org/10.1007/s11998-018-0132-x

Characterization of paint formulated using secondary TiO2

pigments recovered from waste paint
Mikael C. F. Karlsson, Rubén Álvarez-Asencio, Romain Bordes, Anders Larsson, Phil Taylor,
Britt-Marie Steenari

Ó The Author(s) 2018

Abstract The paint industry is continuously striving Keywords Recycling, TiO2, Paint, Waste
to reduce its environmental impact, especially when it
comes to the major virgin white pigment, titanium
dioxide (TiO2). In this work, recycled TiO2 pigment Introduction
was used in a paint formulation as a replacement for
pigment made from virgin raw materials. The paint was Due to its ability to scatter light, titanium dioxide
evaluated based on pH, Stormer and ICI viscosities, (TiO2) is the most widely used white pigment and is
gloss, hiding power, and color characteristics. The paint used in a variety of products such as coatings, paper,
films were also characterized by LVSEM–EDS, AFM, and plastics.1 Minerals that are used in the production
and profilometry. The most significant difference of TiO2, such as ilmenite and raw rutile, are relatively
between a paint based on recycled pigments and a abundant in the earth’s crust2 and do not pose a
paint based on virgin pigments was the agglomeration limitation at the moment. However, the production of
of pigment particles which gave a reduction in gloss pigment grade TiO2 has a high energy demand and
and a rougher surface of the dried paint film based on comes with significant environmental impacts in the
recycled pigment, and it could be concluded that the form of CO2 emissions and large amounts of waste that
recycled pigment could not be used without accepting a need to be handled.3
small decrease in paint quality. This points toward two The paint industry is therefore continuously looking
main directions: (1) the use of recycled pigment in for replacements for TiO2 in order to reduce both the
applications with less demand on surface finish and cost and the environmental impact of their products.4
gloss, such as ceiling paints, and (2) that further work One possible source for a replacement of virgin TiO2
on formulation should be carried out with the recycled could be to recover pigment from waste paint and to
pigment as for any other new pigment introduced in a make it possible to reintroduce the recycled pigment
paint formulation to optimize its performance. into new paint formulations in a circular manner.
In a previous study,5 TiO2 together with a mix of
inorganic extender pigments, mainly dolomite, was
M. C. F. Karlsson (&), R. Bordes, B.-M. Steenari recovered from paint through a pyrolysis-based recy-
Department of Chemistry and Chemical Engineering, cling process. The mix of recycled pigments was then
Chalmers University of Technology, Kemivägen 4, substituted in place of virgin TiO2 pigments in two
412 96 Gothenburg, Sweden different paint formulations. The paints produced with
e-mail: [email protected] recycled pigments showed a decrease in important
qualities, such as whiteness and gloss, compared to
R. Álvarez-Asencio, A. Larsson paints made with virgin material. This decrease in
The Unit of Surface Process and Formulation, RISE quality could be acceptable if it was not for the large
Research Institutes of Sweden, Drottning Kristinas Väg 45, aggregates ( 1 mm in diameter) of TiO2 particles in
114 28 Stockholm, Sweden
the dry paint film.
P. Taylor To be able to study the effects of the recycling
AkzoNobel Decorative Paints Global Research & process on the TiO2 specifically, another study6 was
Development Open Innovation, AkzoNobel Decorative conducted where TiO2 was extracted from a paint
Paints, Wexham Road, Slough, Berkshire SL2 5DS, UK made with TiO2 as the only inorganic pigment. In that
J. Coat. Technol. Res.

investigation, the recycling process was slightly altered Materials and methods
and a washing step was added to remove salt residues
from the recycled pigment. The surface characteristics To evaluate the performance of the recycled pigment6
of the recycled pigment were compared to those of a in a real application, it was incorporated into the paint
virgin pigment, delivered directly from a pigment formulation given in Table 1. This formulation repre-
producer. It was concluded that the recycled pigment sents a general emulsion paint, with the main differ-
had similar properties to the virgin pigment and it ence to a normal paint formulation being that it
would be possible to use in new paint formulations. excludes all pigments other than TiO2. With all other
However, this is not always the case and the specific pigments omitted, the evaluation of the influence of
surface chemistry of TiO2 plays a major role in its TiO2 in the formulation is made easier. All materials
recyclability by pyrolysis.7 used in the paint fabrication, except the recycled TiO2
Paint formulations are complicated mixtures of pigment, were of commercial quality and used as
many different surface active components making it acquired from Akzo Nobel Decorative Paints, UK, and
hard to predict the performance of a recycled pigment Akzo Nobel Performance Additives, SE. The details of
in a paint formulation based solely on the character- the process of producing the recycled pigment and the
istics of the pigment. Therefore, this paper presents the details regarding pigment properties can be found
results from experiments where the recycled pigment, elsewhere.6
produced and characterized by Karlsson et al.,6 was A summary of the pigment properties is given in
used to produce a new paint. The paint properties were Table 2. To homogenize the recycled pigment before
evaluated with conventional methods used by the paint use, the pigment was milled with a ball mill [RJM 103
and coatings industry with the purpose to evaluate the from EnviSense (PL)]. Approximately 350 g of recy-
performance, and to assess the potential use of the cled pigment (roughly 80 mL) was placed in a 1 L
recycled pigment as a replacement for virgin pigments LDPE bottle (outer diameter 95 mm; height 206 mm)
in paint formulations. with 65 stainless steel balls (8 mm in diameter). The
pigment was milled at 300 rpm for 2 h.
The properties of the paint based on recycled
pigment were compared to the properties of a standard
paint with the same formulation but based on virgin
pigment.
The paint was produced with a high-speed impeller
Table 1: Paint formulation used to evaluate both the dispenser from Dispermill Vango 100 from ATP
recycled and virgin TiO2 pigments Engineering (NL) with a dissolver blade of 50 mm in
Raw materials wt% diameter. The mill base was dispersed at 2000–
2500 rpm (peripheral speed of 300–400 m/min) for
Mill base 15 min. The geometry of the dispersing vessel and
Water 22.92 position of the dispenser blade were according to
Antifoam 0.51 guidelines given by Patton.8
Nonionic surfactant 0.51 Properties evaluated on the liquid paints were pH
Anionic surfactant 0.46 and viscosity in the form of Stormer and ICI viscosity,
Hydroxyethylcellulose (HEC) 0.51 while hiding power, gloss, and color characteristics
TiO2 30.47 were measured on dry paint films. All properties were
pH modifier 0.25 evaluated using test methods adopted from standard
Let down methods commonly used by the paint industry. Gen-
Incan preservative 0.12 eral information regarding the test methods can be
Binder (vinyl acrylic) 44.25 found in Ref. 9, while specific details of methods are
Theoretical properties given in sections ‘‘Test methods used on liquid paints’’
Volume % solids 35.5 and ‘‘Test methods used on dry paint films.’’ The dry
Pigment volume concentration 26.4 paint films were also analyzed by atomic force
Density (kg/L) 1.4 microscopy (AFM), environmental scanning electron
microscope coupled with energy diffraction analysis of

Table 2: Properties of pigments used to produce paints for evaluation (adapted from Ref. 6)
Pigment Type Coating Conductivity Specific Particle size Isoelectric point
(10 wt%) surface (in 10 mM NaCl)
D(v,0.1) D(v,0.5) D(v,0.9)

Virgin pigment Rutile Al 0.2 ± 0.1 mS/cm 17 m2/g 0.15 lm 0.28 lm 0.43 lm 7.4
Recycled pigment Rutile Al < 0.001 mS/cm 16 m2/g 0.13 lm 0.27 lm 0.45 lm 7.6
 J. Coat. Technol. Res.

X-rays (low vacuum scanning electron microscopy with Low vacuum scanning electron microscopy
energy-dispersive spectroscopy, LVSEM–EDS) and with energy-dispersive spectroscopy (LVSEM–EDS)
profilometry.
Paints rolled on black Leneta sheets were cut with
scissors to a size of 10 mm by 10 mm and deposited on
Test methods used on liquid paints carbon tape. The samples were then observed with a
FEI Quanta 250 LVSEM operating at 12 kV and
Stormer viscosity was measured in Krebs units (KU) at pressure of 70 Pa. The LVSEM was also coupled to an
room temperature with a Krebs unit viscometer Oxford Instruments energy-dispersive X-ray spec-
(Braive Instruments). ICI viscosity was measured in troscopy (EDS) detector, under the same conditions.
poise (P) measured using a CAP1000 + viscometer Elemental analysis was done on each sample at 2
(CiAB Instruments) at 25°C with spindle number 01 at different positions by area scan (700 9 400 lm).
750 rpm. The pH was measured with a LE 409 pH
electrode connected to a FE20 pH meter (Mettler
Toledo). The electrode was calibrated daily using a 3- Atomic force microscopy (AFM)
point calibration curve with pH standards 4, 7, and 9
(Labservice AB). Stormer viscosity, ICI viscosity, and Nanometer-scale lateral resolution images of surface
pH were all measured 24 h after paint manufacturing. topography and surface nanomechanical properties
To evaluate shelf life, the paints were stored at 50°C were obtained using an atomic force microscope, Mul-
for 5 weeks. After cooling to room temperature, timode, Nanoscope V (BrukerÒ, Santa Barbara, CA),
Stormer viscosity and ICI viscosity were measured. operating in PeakForceÒ QNM mode. A silicon nitride
An ocular inspection was also made of the stored cantilever, ScanAsyst-Air (BrukerÒ, Santa Barbara,
samples to identify any signs of syneresis (liquid/liquid CA), was utilized for all experiments. PeakForceÒ
separation) or settling. Quantitative NanoMechanics (PeakForceÒ QNM) is
an atomic force microscopy mode that provides high-
resolution topography imaging and nanomechanical
Test methods used on dry paint films properties such as adhesion and dissipation.12,13 In this
mode, the scanner oscillates in the normal direction with
Before applications were made for paint film evalua- a frequency in the range 0.5–4 kHz. While scanning, the
tion, the paint samples were filtered through a 125-lm AFM feedback loop keeps the chosen applied force
filter to remove possible residual agglomerates or dry constant (peak force) by correcting the overall extension
paint film. Drawdowns of 150 lm wet film thickness at of the piezo. A force curve is obtained with every tip
a speed of 1500 mm/s were made with an Automatic contact, and its analysis provides the nanomechanical
Film Applicator L (BYK instruments) on black and properties which are displayed in the images. The
white (Form 10B) checkerboard charts (Leneta Com- possibility to apply and control very low forces (pi-
pany). The paint films were stored at room tempera- conewton range) leads to nondestructive imaging.
ture to dry, and then, color characteristics, hiding Drawdowns of the wet paint were made using a 90-
power, and gloss were analyzed. lm film applicator on freshly cleaved mica and allowed
Color characteristics were measured with a CM-600 to dry 24 h at 23° C and 50% RH before observation
handheld spectrophotometer (Konica Minolta) in the with AFM.
L*, a*, b* color space10 with Illuminant D65. The color
difference between paint based on virgin and recycled
pigment is expressed as DE*2000, where the virgin Profilometry
pigment is used as Ref. 11. The hiding power of the
paint films was measured, as the ratio of the reflective The surface texture of the rolled paints was measured
tristimulus Y (CIE) over the black and white parts of using a stylus instrument (DektakXT stylus profiler
the Leneta chart, using a chroma meter (Konica from Bruker), a contacting technique. A diamond tip
Minolta CR-300). Both colorimeters used were cali- with a radius of 2 lm was drawn 10 mm over the
brated to substrates with known color coordinates. surface at a speed of 0.11 mm/s. The distance between
Gloss of the dry paint films was measured at angles 20°, each sampling point was 0.37 lm. The force on the tip
60°, and 85° with a micro-TRI-gloss (BYK Gardner). was set to 0.1 mg. The vertical scan range was set to
Before each measurement, the instrument was cali- 524 lm with a vertical resolution of 8 nm in this work.
brated against the integrated standard that comes with
the instrument.
In addition to the drawdowns, the paints were also Results
applied with a roller (Elite roller set, Anza) for wall
and ceiling applications, on a black Leneta sheet. Both In this section, the results of the measurements for the
paints were applied with a calculated wet film thickness paints based on virgin and recycled pigments are
of 200–300 lm in two layers. presented. In general, the results of the absolute
J. Coat. Technol. Res.

measurement values are of minor interest, while the However, before these measurements were taken,
relative difference between the two paint samples is of ultrasound was applied to the pigment suspensions
major importance. and the measurements were taken on a small sample
size (< 0.1 wt% of the total amount used to produce
the paint). Surface characterization of the pigments6
Liquid paint did not indicate any major differences in surface
chemistry between the pigments. Furthermore, the
Both paint samples (using recycled and virgin pig- properties of the paints after the stability test (Table 3)
ments, respectively) yielded the same measured pH do not suggest that there was a problem with the
value of 9.1 ± 0.1. This falls within the range of what colloidal stability of either paint. Therefore, the most
was expected for an emulsion paint. The recycled likely reason for aggregates in the paint based on
pigment did not show any impact on the pH of the recycled pigment is the pigments aggregated during the
paint. recycling process. The shear forces in the milling of the
The results from the viscosity measurements can be paint during manufacturing were not sufficient to de-
found in Table 3. There was a slight variation in the agglomerate the recycled pigment.
ICI viscosity, but the differences were too small to
have a relevant impact on the paint. The difference in
Stormer viscosity between the samples before storage, Low vacuum scanning electron microscopy
110 KU for virgin and 104 KU for recycled pigment, is with energy-dispersive spectroscopy (LVSEM–EDS)
not substantial but may be noticeable for a professional
painter. However, the difference in Stormer viscosity SEM micrographs for paint films using virgin and
may be corrected by adjusting the thickener concen- recycled TiO2 pigments are shown in Fig. 1. A com-
tration in the paint formulation.
Both samples show a slight decrease in Stormer
viscosity after storage. It is not unusual to get slight Table 4: L*, a*, and b* values for paints based on virgin
changes in viscosity after stability testing. Major and recycled pigments
changes in viscosity, syneresis, or gel formation would Virgin pigment Recycled pigment
be a reason for concern, but none were observed for
the paint samples presented here. L* 97.28 96.85
a* 0.82 0.63
b* 1.08 1.42
Dry paint DE2000 Reference 0.51

The color coordinates for the two paint films are

presented in Table 4. The color difference between the
two films is summed up to DE2000 = 0.51. This Table 5: Hiding power measured in the form of contrast
difference is on the limit of what the human eye can ratio Yw/Yb of paints based on virgin and recycled
detect,9 and for many practical applications, this pigments, where Yw and Yb represent the measurement
difference is acceptable. value on white and black background, respectively
The recycled pigment gave a slight decrease in
hiding power compared to the virgin pigment as shown Virgin pigment Recycled pigment
in Table 5. This, combined with the significant
Contrast ratio 98.1 ± 0.3% 97.3 ± 0.5%
decrease in gloss (Table 5), suggests that the recycled
Gloss 20° 32.4 ± 1.1 5.3 ± 0.5
TiO2 was aggregated, thus not having the right particle
Gloss 60° 73.5 ± 2.4 22.0 ± 1.9
size distribution for optimum light scattering.
Gloss 85° 92.0 ± 7.4 17.3 ± 1.4
The particle size measurements that were made
previously6 did not suggest that the recycled pigment Gloss measured in angles 20°, 60°, and 85° to the paint film.
was more aggregated than its virgin counterpart. Uncertainty of measurement given as one standard deviation

Table 3: Viscosity values of paint samples based on virgin and recycled paints, respectively
Sample 24 h after fabrication After stability test
Virgin pigment Recycled pigment Virgin pigment Recycled pigment

Stormer [KU] 110 ± 2 104 ± 2 106 ± 2 102 ± 2

ICI [P] 0.59 ± 0.09 0.65 ± 0.10 0.63 ± 0.12 0.70 ± 0.11
Samples were measured 24 h after fabrication and after stability test (5 weeks in 50 °C). Uncertainty of measurement given as
one standard deviation
 J. Coat. Technol. Res.

parison of the micrographs revealed a substantial aggregates in the paint made with recycled pigment
difference between the paint based on the virgin with the largest aggregates being approximately
pigment and the paint containing the recycled pigment. 100 lm in diameter. For both paint films, three major
Paint film using the virgin pigment (Fig. 1a) is rather components were detected (C, O, and Ti) in the EDS
smooth, whereas Fig. 1b confirms the formation of analysis. The average atomic ratio of the paint film

Fig. 1: Micrographs of paint using (a) virgin pigment and (b) recycled pigment. 503 magnification

(a) (b)

200.0 nm 3.0 nN

– 50.0 nm
0.0

Height 400.0 nm
Adhesion 400.0 nm
(c) (d)

200.0 nm 3.0 nN

– 50.0 nm 0.0

Height 400.0 nm Adhesion 400.0 nm

Fig. 2: AFM of paint film based on virgin and recycled pigments. (a) Topography, (b) adhesion for virgin pigment, (c)
topography, and (d) adhesion for recycled pigment. Light is up and dark is down in the topographic image, and light is high
adhesion, while dark is low adhesion in the adhesion image
J. Coat. Technol. Res.

based on virgin pigment was 48% C, 40% O, and 10% Profilometry

Ti, while the paint film based on recycled pigment had
an average composition of 51% C, 39% O, and 10% Ti. The surface structure and roughness of the hand-rolled
This leads to the conclusion that there was no virgin pigment- and recycled pigment-based paint films
significant difference between the paints regarding are shown in Fig. 3. Compared to AFM, profilometry
the atomic composition or spatial distribution of the looks at a larger scale, more relevant for the visual
atoms. appearance of the films. For both paint films shown in
Figs. 3a–3b, the surface structure was fairly rough with
hills and valleys up to 100 lm apart. Both types of
Atomic force microscopy (AFM) paint show a long waviness profile which comes from
the application method of using a hand roller aimed at
The microstructure and adhesion were investigated by producing this effect. The finer waviness (noise)
AFM using a PeakForce QNM mode on the paint film referred to as roughness is shown in Fig. 3b for the
surface for paints based on virgin and recycled recycled pigment-based paint film but is absent on the
pigments as shown in Fig. 2. From the height images surface profile of the virgin pigment-based paint
(Fig. 2a and 2c), little difference could be observed, (Fig. 3a).
except maybe a slightly rougher character in the case of The separation of waviness from roughness was
the films based on recycled pigment. The topographic achieved using Vision64 version 5.51 update 2 soft-
images are slightly blurred; this is most likely due to ware. The primary profiles for each paint from Figs.
the thin layer of surfactant covering the surface of the 3a–3b were filtered so that waves longer than 0.5 mm
paint films as suggested by the adhesion micrograph (called waviness) were removed, while waves shorter
(Fig. 2b and 2d). Below the surfactant is the more than 0.5 mm (called roughness) were displayed. The
adhesive latex film (data not shown). This was filtered profiles are shown in Figs. 3c–3d for virgin
expected considering the paint formulations were the pigment- and recycled pigment-based paints. It be-
same except that the pigment was changed. Interest- comes clear that the roughness of the paint with the
ingly, no difference could be seen for the adhesion recycled pigment is much larger than that of the virgin
pictures (Fig. 2b and 2d). The dark areas correspond to pigment. However, the surface structure of the appli-
low adhesion in the adhesion images. These areas are cation method is more dominant to the overall paint
likely to be the TiO2 pigment which appears (on this structure than the contribution of the aggregated
length scale) to be well distributed throughout the pigments. This, together with the size of the aggregates
paints. (see Fig. 1), makes the agglomerates hard to detect for

Virgin Recycled
(a) 60 (b) 60

40 40
(Height/ µm)
(Height/ µm)

20 20

0 0

-20 -20

-40 -40
0 2 4 6 8 10 0 2 4 6 8 10
(Length/ mm) (Length/ mm)
(c) 60 (d) 60
(Height/ µm)
(Height/ µm)

40 40
20 20
0 0
-20 -20
-40 -40
0 2 4 6 8 10 0 2 4 6 8 10
(Length/ mm) (Length/ mm)

Fig. 3: Primary line scan of the stylus profilometer. (a) Virgin pigment-based paint film and (b) recycled pigment-based
paint film. Surface roughness of the line scan for (c) virgin pigment-based paint film and (d) recycled pigment-based paint
film. Each line scan is 10 mm in length
 J. Coat. Technol. Res.

an observer at a distance beyond 30 cm from the paint the agglomerates due to the topography of the rolled
film. paint. Furthermore, the gloss of the formulation based
on recycled pigments was higher than that on most wall
and ceiling paints, so an extender pigment would be
Concluding remarks needed to reduce the gloss even further. This means
that the recycled pigment might be of greater value in
Two paint formulations were compared in this re- formulations with lower gloss or sheen, which is one
search. One paint formulation was based on virgin of the currently developing trends in the global
TiO2 pigment as received from the supplier, while the decorative paint market. Additionally, the paint based
other paint formulation was based on recycled TiO2 on recycled pigment could be applied to rough
pigment. All other paint components were kept con- surfaces, such as a mineral substrate, without any
stant in order to compare and evaluate the perfor- problems. One other application for the paint could
mance of the recycled TiO2 pigment when compared to be surfaces that usually do not get scrutinized
the virgin TiO2 pigment. carefully, such as ceilings.
The Stormer and ICI viscosities as well as the pH In the formulation presented in this work, 100%
were measured on liquid paints. There were no replacement of virgin pigment with recycled pigment
significant differences in pH or ICI viscosity between was done. A smaller replacement would most likely
the paints based on either virgin or recycled pigment. have less impact on the paint properties. If the recycled
The liquid paints only showed a small difference in pigment is not used as a replacement for TiO2 pigment
Stormer viscosity, which was deemed acceptable and in a high gloss paint formulation, it could be used as a
could be adjusted by the addition of a thickener. so called extender or filler pigment. Extender pigments
The dry paint films were evaluated based on the are used to reduce gloss in, for example, formulations
color difference, hiding power, and gloss. The slight for wall and ceiling paints. Here, the recycled pigment
difference in color between the two paint films is would have the benefit of reducing gloss without the
insignificant for most applications. However, the paint trade-off in reduced whiteness or opacity which is
based on recycled pigment had a lower hiding power normally associated with more traditional extender
than the paint based on virgin pigment. One of the pigments.
main reasons TiO2 is used as a pigment is due to its Overall, the results of the present investigation show
ability to produce white paints having a very good that it is possible to recycle TiO2 pigments from paint
hiding power or ability to scatter light. Even though waste, with minor effects on the appearance. However,
there is a slightly lower hiding power for the paint the gloss and covering power of the recycled pigment
based on recycled pigment compared to the virgin were lower than those of paint made with the virgin
pigment, it is the reduction in gloss that is the bigger pigment due to pigment aggregation. Agglomeration
issue. The reduction in gloss turns the formulation could probably be mended by further work on formu-
from a glossy (virgin pigment) to a mid-sheen formu- lation, which is expected to be done as for any new
lation (recycled pigment). pigment product. The performance of the recycled
The surface structure and morphology of the dry pigment was deemed as clearly promising by the paint
paint films were also analyzed using AFM, LVSEM– industry which motivates further development in the
EDS and profilometry. The presence of aggregates was field.
visible in the drawdowns. A previous study,6 showed
no significant difference between virgin and recycled Acknowledgments The authors acknowledge
pigments in particle size or surface characteristics. It is, financial support from the Swedish Governmental
however, impossible to rule out that minor alteration Agency for Innovation Systems (Grant number:
has occurred at the surface of the recycled pigment in P37547-1), Akzo Nobel Decorative Paints, UK, and
terms of surface chemistry. This alteration would play a Stena Metal AB, Sweden. Work was partly financed by
role when it comes to the interaction with the surface scholarship granted from the Swedish Paint and
active components of a paint leading to aggregation, Printing Ink Makers Association and the Swedish
for instance during film forming. This observation also Adhesive and Sealants Association. The authors would
suggests that the formulation of paint should be tuned especially like to thank the personnel at Akzo Nobel
toward the use of recycled pigment, as for any other Performance Additives SE for their support.
pigment. It should also be mentioned that, due to the
rough surface, the durability of the paint film based on Open Access This article is distributed under the
recycled pigment could be reduced compared to when terms of the Creative Commons Attribution 4.0
using virgin pigment. International License (http://creativecommons.org/lice
Even though the recycled pigment gives a quality nses/by/4.0/), which permits unrestricted use, distribu-
decrease, its use remains largely possible. In certain tion, and reproduction in any medium, provided you
applications, this drop in performance can be accept- give appropriate credit to the original author(s) and
able. When the paint containing the recycled pigment the source, provide a link to the Creative Commons
was applied with a roller, it was very hard to identify license, and indicate if changes were made.
J. Coat. Technol. Res.

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