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Handbook of Solvents - George Wypych - ChemTech - Ventech!

Handbook of Solvents - George Wypych - ChemTech - Ventech!

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396 Seung Su Kim, Jae Chun Hyun<br />

7.3.3 MEASUREMENT OF THE DRYING RATE OF COATED FILM<br />

The drying rate <strong>of</strong> coating is easily measured by simple experimental equipment. In a controlled<br />

air condition, the weight loss <strong>of</strong> coating due to the solvent evaporation is measured<br />

by electrical balance and filed at the PC. The weight loss with time is converted to drying<br />

rate <strong>of</strong> coating per unit area. The commercialized experiment equipment is commonly used<br />

to obtain the drying rate, such as thermo-gravimetric analyzer (TGA). Nowadays commercial<br />

TGA equipped with FT-IR or gas chromatography is available and readily used to obtain<br />

not only the overall drying rates <strong>of</strong> coatings but also the relative drying rate <strong>of</strong> each<br />

solvent in a multi-solvent system. However it is difficult to obtain such data at a high air velocity,<br />

because the air stream disturbs the balance and cause to oscillate the balance reading.<br />

Practically the available air velocity <strong>of</strong> this kind would be 1 m/sec or lower.<br />

Fourier-Transform-Infrared (FT-IR) spectrometer is used to obtain the drying rate at a<br />

higher air velocities. 47,50 FT-IR is commonly used for the analysis <strong>of</strong> organic materials. Recently,<br />

FT-IR is applied to measure the drying rate <strong>of</strong> coating. This specially designed<br />

FT-IR with coating apparatus and air blowing system made it possible to measure solvent<br />

content without disturbances <strong>of</strong> airflow, and moreover it enabled us to find the content <strong>of</strong><br />

each solvent with drying proceeded. 47,50 This can be used to study selective evaporation <strong>of</strong><br />

solvent and phase separation phenomena in a multi-solvent system. 50<br />

The air velocity <strong>of</strong> industrial dryer is up to 20 m/s or more and the temperature <strong>of</strong> oven<br />

is normally up to 200 o C. A specially designed drying chamber was suggested to measure<br />

solvent concentration in these drying conditions. 52,57 The chamber is equipped with flame<br />

ionization detector (FID) total hydrocarbon analyzer, and the oven exit gas which contains<br />

the evaporated solvent flows to the analyzer. The drying rate is calculated by multiplying<br />

the solvent concentration with exit gas flow rate. It provides access to a wider range <strong>of</strong> drying<br />

conditions that approximate industrial conditions.<br />

However, it is much more difficult to find out the actual drying rate <strong>of</strong> coating in an industrial<br />

dryer. In a continuous industrial dryer it is impossible to measure the drying rate by<br />

any <strong>of</strong> the above methods, because the coated substrate is running through the dryer at the<br />

speed <strong>of</strong> several hundreds meter per minute. To measure the drying rate <strong>of</strong> coating in such a<br />

condition, the dryer exit gas <strong>of</strong> each zone is analyzed by gas chromatography. Then the drying<br />

rate <strong>of</strong> each zone is calculated by multiplying solvent concentration with exit gas flow<br />

rate. From the drying rate <strong>of</strong> each zone, the evaporated amount <strong>of</strong> solvent is calculated. Thus<br />

the solvent concentration <strong>of</strong> coating is found at the point <strong>of</strong> each zone end. 28,30<br />

7.3.3.1 Thermogravimetric analysis<br />

The drying rate <strong>of</strong> a coating could be easily found by measuring coating weight loss during<br />

drying in a laboratory. The set-up <strong>of</strong> experimental equipment is relatively easy, and the<br />

commercial equipment can be readily available such as thermogravimetric analyzer<br />

(TGA). 5,53 As drying proceeded, the weight <strong>of</strong> coating decreases due to the solvent evaporation.<br />

The amount <strong>of</strong> solvent loss with time is monitored by the balance. The schematic representation<br />

<strong>of</strong> the equipment is shown in Figure 7.3.10. The sample, such as coated films or<br />

a tray that contains the coating liquid, is mounted on the balance to be monitored. The temperature<br />

<strong>of</strong> coating is measured by non-contact infrared thermometer. A thin wire type thermocouple<br />

can be used to measure the temperature, and the thermocouple is attached to the<br />

coating or sample tray. The air is made up by conventional blower and is heated up to a certain<br />

temperature by electrical heater. The air is supplied to the coating surface through

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