rheological studies of the cure of epoxy/polyester powder coatings containing titanium dioxide. - characteristics of polyester
The curing properties of a series of powder coatings containing titanium dioxide dispersed in epoxy/polyester matrix are reported.
Titanium dioxide pigment is produced through two ways of chloride and sulfuric acid, coated with different amounts of aluminum and silica.
Comparison data for preparations containing zinc oxide and silica are also included.
The gel time of these powder coatings depends on many factors.
Increasing the level of the flow agent significantly shortens the time for gel.
In the case of sulfuric acid, the presence of trace zinc inhibits curingbased pigments.
Changes in the content of alumina and silica in the titanium dioxide redox coating also affect the time of gel.
Increase silica content on chlorine-
The base coating increases the time of gel, while in the case of sulfuric acid based coating, the time of gel is shortened.
These differences are attributed to the effect of zinc in the coating and the effectiveness of the diammonium catalyst.
Strathclyde rheometers, titanium dioxide, zinc oxide, silica, epoxy polyester, Modaflow, titanium dioxide containing powder coatings are widely used in white home appliance manufacturing due to its environmental protection and basically zero solvent emissions. (1-5)
Although the appearance of the coating is the only important factor for many applications, it has been shown that the curing conditions will affect the corrosion properties of the epoxy polyester powder coating. (6)
The protective properties of the coating are affected by the cross-linking density of the formed substrate.
The addition of titanium dioxide in epoxy polyester powder coating will affect the curing properties. (7)
Properties of powder curing
Interesting challenges are presented based on the system. (8)
Usually, curing state can be studied by spectral and differential scanning heat, and these technologies have been widely used in the study of powder coatings. (9-11)
The process of powder coating usually involves spraying a preheated item with a heated powder and then melting it by heating.
Curing is caused by melting the powder on the covered item and will be affected by the substrate thermal capacity, heating temperature, amount of powder deposited and the speed of cooling the item.
In this article, the influence of titanium dioxide composition on the surface of epoxy polyester powder coating was studied using Rheometric measurements.
The curing in the hot solid resin is monitored by observing the change of viscosity over time. (12)
Strathderderheometer has the ability to study the high-filled polymer system and is very suitable for the Study of powder coatings. (13), (14)
Titanium dioxide with ruititanium and ruititanium (9), (15);
However, it is often used for the manufacture of pigments in the form of TiO 2.
The red-titanium-type structure is preferred by the Red-titanium type because its high refractive index provides better hiding power.
Two routes are usually used in the manufacture of theTi [O. sub. 2]
These are sulfuric acid and chloride.
Sulfateroute includes the extraction of titanium from the original ore using sulfuric acid, followed by hydrolysis and calcification.
It can be produced by controlling the hydrolysis and calcification process materials with different impurity levels and particle sizes.
The chloride process involves the treatment of the ore with the gas chlorine that forms the titan, and then hydrolysis and calcification to produce the particles of the required particle size.
In this studyO. sub. 2]
Two methods were studied. The Ti[O. sub. 2]
Particles used as pigments are stabilized by coating with alumina and silica.
This coating inhibits the light activity of Ti [O. sub. 2]
Particles and block free radical generation that may cause degradation of the coating.
A series of alumina variable capacity pigments--
The silica content was created for this study.
The purpose of this study is to determine the possible connection between "the method of producing titanium dioxide pigment particles and their effect on the curing process.
The curing process was studied, and the rheometers of Clyde were determined. (13), (14)
Curing of epoxy resin is the subject of extensive research over the years and has published many detailed papers covering discussions on dynamics, curing mechanism and in-situ monitoring techniques.
This article focuses on the solidification of Ti [by means of a biomechanical measurement]O. sub. 2]
, Colored powder paint. (16-24)
Experimental material titanium dioxide pigment is a research grade material provided by the Research Laboratory of the ICI Center of Stocktonon-Tees.
Table 1 summarizes the features of these materials.
The pigment is made of chlorine. A]and sulfate [B]processes.
The two basic pigments are coated with different amounts of silica and alumina.
The composition of the pigment was determined by x-
I'm from zinc oxide.
% Levels exist in the Sulfateroute material, added as a crystal stabilizer and reduced the photoactivity of the final pigment.
Series A pigments do not have any detectable zinc content. X-
The composition of the elements on the surface of the pigment was determined by X-ray electron spectroscopy. Table 2.
XP stechnique allows to distinguish between elements in bulk and on the surface of particles.
The spectrum is recorded on the instrument described earlier. (16)
The spectrum is referenced to a carbon peak of 285 eV.
Peakswere of Ti 2 [observed]p. sub. 3/2], Zn 2[p. sub. 3/2]
, Al 2 p, Si 2 s and O Is, their assignment Is consistent with the values previously referenced in the literature. (25), (26)
Comparison of data in table 1 and Table 2 shows that the concentration of zinc in Series B pigments is low.
The amount of ZnOfound found in Series B depends on the temperature of the calcium.
The electron microscope shows that the pigment particles are similar in size and are consistent with the previous observations ,(25)Fig. 1.
Representative electronic micrographs of pigments A2 and b2 are introduced. [
Figure 1 slightly]
Thickness of silica--
The Alumina coating varies from particle to particle with a thickness of about 10 nm but is not completely uniform.
Analysis of the surface using EDAX shows that each component of the coating appears to retain its own personal structure and exist as an area of silica or alumina.
The fiber structure on the surface of some pigments is rubber-like silica, and alumina forms closer spots.
The average size of the particles determined according to the electronic microscopic photos is ~ 220 nmA]
The wavelength of sulfuric acid route pigment is about 230 nmB]. X-
X-ray deposition analysis shows that the particle size of chlorine route pigments varies from 100 nm to 500 nm, and the particle size of sulfuric acid varies from 20 to 500 nm. based pigments.
Although the form of distribution granularity is slightly different, the size of the pigment is comparable.
The typical particle size is shown by a and Bpigments. 2.
The average particle size of type A and Type B pigments is ~ 0. 3 [micro]n.
There was no significant difference in particle size distribution of pigments used in this study. [
Surface area the surface area of the pigment is determined using nitrogen measurements, table 3. The silica-
Compared with undeposited pigments, the Alumina coating significantly increases the surface area of the particles--A1 and B1.
Surface acidity is studied by non-drop method n-
Determine the end point with Hammett indicator. (20)
No significant color changes were found, indicating that the coating process did not introduce significant acidity and alkalinity to the particles.
Two other pigments were examined by other pigments: zinc oxide and silica.
Zinc oxide was obtained from Durham Chemical Co. , Ltd.
Surface area of 8 【m. sub. 2][g. sub. 1]
The average particle size is 1. 4 tm.
Silicon obtained from crotsfield Chemical Co. , Ltd.
The surface area is 750 [m. sub. 2][g. sub. -1]
The average particle size is 4. 5 rim.
The resin used in this study was prepared from the double phenol monodidinyl ether resin.
Epikote 1055 from Shell UK Chemical Co. Ltd.
, As well as the end amino polyester provided by the British DSM.
The soft sign value of epoxy resin is 850 and the soft sign value is 94 [degrees]
C and aviscosity of 450 cPs, as 40% solution in positive carbon alcohol at25 [degrees]C.
The acid value of polyester Uralac P2347 is 75-
90, the glass transition temperature is 54 [degrees]
C and viscosity are between 100 and 200 cPs at 165 [degrees].
To help disperse the pigment in the resin, Modallow was used.
Modallow is obtained from Monsanto and is an acrylic-2-
Acrylic acetate ester.
Table 4 provides an overview of the molecular weight features of the materials obtained by gel penetration chromatography operating with sifluoride as a solvent.
Formulation of powder coatings epoxy and polyester powders are mixed in a chemical metering ratio (704 g/542 g)
Additive with flow rate (Modaflow)
In the main batch of 6 episodes. 2 g.
Variables were added to the main batch.
Initial mixing is performed in a water cooled Henschel mixer for 5 minutes and a uniform premix is produced.
Extrusion of premix using buss pr 46 single screw extruder the working temperature of this extruder is 100 [degrees]
C and screw temperature of 30 [degrees]
C and mold temperature 80 [degrees]
C and throughput 9-10 kg [h. sup. -1].
The extrusion is ground using a pin Disc mill to obtain a powder with a particle size [less than]125 pm.
Methods the curing process of powder was studied with Strathclyde.
The rheometer uses a vibrating probe to detect changes in the viscosity of the material and has previously been shown to be well suited for the Study of filling polymer systems. (27), (30)
The instrument works at a frequency of 1Hz.
Place the powder sample in a glass container with a diameter of 2 cm and heat it in an oil bath.
All measurements were made at 140 [degrees]C.
The viscosity distribution is calculated using the amplitude and phase output of the phase signal.
The theory proposed before use (12)
The viscosity time distribution is calculated.
[Viscosity]10. sub. 4]
Pa is considered as an indication of the gel of the material, which is related to the data obtained from other methods and the point at which the gel occurs. (12)
Results and discussion a series of measurements were made using formulas created using pigments and ingredients summarized in Table 1.
In order to set the baseline, the resin system was measured without adding titanium dioxide.
Before exploring the effect of Ti [s], the influence of the flow measurement of Modaflow on the curing process0. sub. 2]
In the course of treatment.
The formulation of modaflow at different concentrations was measured to determine the effect of the dispersing agent on gel time.
Modaflow is acrylic acetate-2-
The ethyl hexyl acrylatecopolymer, but also contains the aromatic acid function that may enter the curing reaction of epoxy resin.
The viscosity traces are shown in Figure 1. 3.
The addition of Modaflow shortens the curing time when hut reaches the saturation level at 0. 5% w/w.
Modaflow may have two effects on the healing process.
First, it can locally increase the catalyst to make the composition more reactive to his achievements; secondly, it can participate in the curing process through the itscarboxyl acid function.
The formula containing 0 is studied. 5% w/w of di-2-
Ethyl hexyl ester. Di-2-ethylhexyl-
Sebacate is structurally similar to Modaflow but does not contain any reactivate acid function.
Curing curve obtained2-
Acetate is the same as 0.
5% w/w Modaflow, figure3.
This means that the acceleration of the curing process is-
Instead of introducing additional chemical reactivity to the system. [
Figure 3 slightly]Effect of Ti[O. sub. 2]
Grade of ten different titanium in curing process [O. sub. 2]
The formula for the production of pigments, table 1 and powder coatings is the use of 3.
3% w/w pigment and 0.
5% w/wof Modaflow.
As a reference, the traces of theModaflow were also measured for each pigment in the resin mixture in the resin system. system.
The curing curves of these formulas are shown in the figure4. [
Figure 4 slightly]
Series A preparations are produced using A chlorine route, which is free of zinc, while Series B preparations are obtained through A sulfuric acid route, containing about 1% w/w of zinc.
As mentioned earlier, changing the properties of silica/Alumina Coatings on titanium dioxide pigments has no effect on the curing process.
The time for gel at the point where the viscosity reaches [value]10. sub. 4]
Pas can be drawn according to the ratio of silicon to aluminum determined by XPS analysis, fig. 5.
The behavior of Series A and Series B is significantly different.
In the case of the zinc freeA series, the increase in the ratio of silicon to aluminum increases the time. [
Figure 5 Slightly]
Silicon dioxide may produce Lewis acid sites, and mixed Silicon-aluminum coatings can have both acid and alkali sites at the same time. (31-41)
The acid site has the ability to absorb amine containing organic molecules, thus interacting with DICY.
In the case of zinc-free pigments, increasing the silica content seems to inhibit the curing process, because adsorption on the Lewis acid sites associated with the silica coating on Ti [may result in DICY's0. sub. 2]
In Series B, pigments contain zinc in the form of oxides or ions, and an increase in the ratio of silicon to alumina results in a decrease in gel time.
In systems containing titanium and silica, the adsorption of amine at acidic sites has been observed in Amine curing studies of epoxy resin (40)
The triacetate amine on γ-alumina was studied. (41)
It is also noted that the B-series pigments are generally longer than the gel time of the-series pigments.
The only major difference between these two series of pigments is the zinc used in series B pigments as a crystal stabilizer.
X-ray fluorescence measurements that provide a large amount of elemental analysis indicate that 1% w/w of the pigment is zinc.
However, XPS, as a surface technique, indicates that there is a very low but limited zinc or zinc oxide present on the surface, table 2.
Double ammonium for epoxy resin system [curingDICY-[(N[H. sub. 2])sub. 2]C=N-C=N].
As we all know, DICY is very sensitive to the existence of zinc, and there is a strong interaction between zinc and zinc. acts. (42-47)
However, DICY is reduced by reacting with metal zinc instead of zinc oxide, just like copper, it can form a complex without changing the structure and reactivity of DICY(47), (48)
Data as shown in the figure
5 means that zinc or zinc oxide can be contacted on the surface of the pigment and can inhibit the curing process of the B series pigment by reaction or adsorption.
Another explanation may be that zinc in bulk produces active titanium sites on the surface.
Further studies are needed to accurately determine the way in which changes in pigment types affect the sex. (36)
The increase in silica levels in Series B can offset the inhibition of zinc and lead to a decrease in gel time.
In order to explore the role of zinc oxide in Series B pigments, zinc oxide was studied as a pigment.
The effect of zinc oxide on curing behavior has previously been reported that the addition of zinc oxide to epoxy/polyester powder coating can be catalytic or inhibit curing behavior. (49)
A series of recipes were created in which the concentration of zinc oxide was changed and the curing properties were measured, fig. 6 [
Figure 6 slightly]
It is reported that non-Hydrated metal oxides can be considered acidic, and XPS studies of epoxy/DICY adhesive systems have found the presence of additional peaks. (50-52)
It was also observed that at low temperatures, zinc compounds can cause changes in diammonides, which are usually associated with high-temperature degradation processes, and lead to the formation of diammonides.
This conversion reaction can inhibit the reaction between dioxamine and epoxy resin and the formation of oxadiol structure, which is the pioneer of the start of the curing reaction.
Adding 5% w/w of zinc oxide can double the gel time.
However, further addition of zinc oxide can lead to a decrease in gel time.
It is clear that the zinc oxide interacts with DICY to inhibit the reaction, but to a certain extent or more, it itself begins the catalytic reaction, which is observed as a decrease in gel time.
This behavior reflects the possible complexity of the interaction with dicy, where zinc has the ability to inhibit curing, while oxide has the ability to inhibit curing by adsorption or acid generation catalysis.
In the case of Series B pigments, it is a zinc oxide of Ti [O. sub. 2]
Suppress the cured surface relative to the pigment.
Effects of silica on curing behavior a study on the effects of silica on the curing process and data on preparations containing different concentrations of si [0. sub. 2]
As shown in the figure. 7.
Adding silica to the formula has a significant delaying effect, increasing the curing time of the resin system from about 40 minutes to 250 minutes.
Silica may be thought to have a strong interaction with DICY and inhibit its ability to catalytic the curing process.
Silica particles can contain surface adsorption sites, which effectively inhibit the absorption of DICY during curing. [
Figure 7 Slightly]Effect of Ti[O. sub. 2]
In order to understand the effect of the surface on DICY initiation curing capacity, the effect of changing Ti [concentration] was investigatedO. sub. 2]
Gel time, figure. 8.
Pigment A4 was used in this study.
Increasing the filler load will result in an increase in gel time from 3 w/w to 6% w/w, however, a further increase in pigment levels will result in a decrease in gel time.
At the highest load, the critical pigment volume is close.
The increase in pigment content increases the interaction between the cured resin and the pigment, resulting in a decrease in gel time. [
Conclusion The study of the flow changes occurring during the curing process of epoxy polyester cured with DICY and filled with various pigments shows that the addition is as high as 0.
The cure rate can be improved by 5% of Modaflow.
Add Modaflow to the formula as a dispersing agent for the filler, but also have the ability to improve the curing rate.
There is a difference between pigments generated using green mud and sulfuric acid routes.
The pigment is coated with a mixture of aluminum and silica, and the comparison of pigments from the common synthetic route shows that the surface coating affects the curing rate.
For zinc-free pigments in the chloride route, an increase in the ratio of silicon to aluminum leads to an increase in curing time.
In contrast, pigments from the sulfuric acid route show an increase in curing time as the ratio of silicon to aluminum increases.
The main difference between chlorine and sulfuric acid route is the growth of seed pigments using zincoxide.
A study using zinc oxide pigments has shown that zinc oxide can accelerate curing and shorten gel time.
Therefore, the difference between chlorine and sulfuric acid pigments is explained to some extent by the possible impact of the accelerated curing process of oxide zinc.
A study using silica pigments confirmed the significance of the study of the effect of coating changes on titanium dioxide pigments, that is, silica can inhibit curing and significantly increase gel time.
Although zinc oxide can inhibit curing, it can promote curing in Series B pigments in combination with silica.
An author (ECT)
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Pethrick * WestCHEM, Department of Pure Chemistry and Applied Chemistry, University of Strathclyde, Thomas Graham Building, 295 GI1X1 Cathedral Street, Glasgow, UKmail: r. a. Perschick @ Strasac. uk DOI 10. 1007/s11998-012-9417-