Method for producing organic solvent solution of quaternary ammonium hydroxide
A technology of quaternary ammonium hydroxide and organic solvent, which is applied in the field of semiconductor manufacturing treatment liquid composition and its manufacturing, and can solve the problems such as not easy to remove
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[0248] Hereinafter, the present invention will be described in more detail using examples and comparative examples. However, the following examples are merely examples for explaining the present invention, and the present invention is not limited to these examples.
[0249] (test methods)
[0250] In Examples and Comparative Examples, the concentration of the quaternary ammonium hydroxide in the solution was measured by potentiometric titration using a potentiometric automatic titration device AT-610 (manufactured by Kyoto Denshi Kogyo Co., Ltd.).
[0251] The amount of moisture in the resulting solution was obtained by correcting the value measured by Karl Fischer titration using a calibration curve. The measurement of the water content by Karl Fischer titration was performed using a Karl Fischer moisture meter MKA-510 (manufactured by Kyoto Denshi Kogyo Co., Ltd.). The measurement of the water content by gas chromatography (hereinafter sometimes referred to as "GC") uses a...
Embodiment 1
[0282] By using apparatus A (thin film distillation apparatus 10A ( figure 1 )) to perform thin film distillation (step (a)), thereby producing an organic solvent solution of quaternary ammonium hydroxide.
[0283] The pipes of the device were disassembled, cleaned and assembled in advance, and cleaned by alternately flowing twice each of TMAH aqueous solution having a TMAH concentration of 25% by mass and ultrapure water (step (b)).
[0284]A raw material mixture prepared by mixing 4 kg of 25% by mass TMAH aqueous solution and 16 kg of PG in a clean bucket made of PE was put into a raw material container made of PE (the mixing mass ratio of aqueous TMAH / PG=1 / 4). The temperature of the raw material mixture just before being dropped into the distillation vessel is 23°C, the temperature (heat medium temperature) of the heating surface of the evaporation vessel is 100°C, the degree of vacuum is 600Pa, and the feed rate is 10.0kg / hour (the temperature of the heating surface) Fee...
Embodiment 2
[0286] Use device A (thin film distillation device 10A ( figure 1 )) and perform the same device cleaning as in Example 1 (step (b)), and then perform thin-film distillation (step (a)), thereby producing an organic solvent solution of quaternary ammonium hydroxide.
[0287] A raw material mixture prepared by mixing 4 kg of 25% by mass TMAH aqueous solution and 16 kg of PG in a clean bucket made of PE was put into a raw material container made of PE (the mixing mass ratio of aqueous TMAH / PG=1 / 4). The temperature of the raw material mixture just before being dropped into the distillation vessel is 23° C., the temperature (heat medium temperature) of the heating surface of the evaporation vessel is 105° C., the degree of vacuum is 500 Pa, and the feed rate is 7.0 kg / hour (heating surface temperature). Feed rate per unit area: 70kg / h m 2 ) under the conditions of thin film distillation, thus obtaining a PG solution (about 4 kg) containing TMAH in the residue liquid recovery cont...
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