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ChemicalBook CAS DataBase List Formaldehyde

Formaldehyde synthesis

13synthesis methods
Formalin is adjusted to pH 8 and urea is added to give a urea to formaldehyde ratio of about 1 :2.5 molar. The resulting solution is boiled under reflux for 1 hour. Butanol (1.5-2.0 mole per mole of urea) is then added together with a little xylene. The latter forms, with butanol and water, a ternary azeotrope which on distillation yields a condensate separating into an upper organic layer and a lower aqueous layer. By discarding the lower layer and returning the upper layer to the reactor, water is progressively removed from the system. After a substantial proportion of the water has been removed, an acid catalyst (e.g. phosphoric acid or phthalic anhydride) is added and heating is continued. When the required degree of reaction is attained, the solution is neutralized and concentrated to the desired solids content.
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Yield:141-46-8 614 μmol ,64-18-6 421 μmol ,50-00-0 158 μmol

Reaction Conditions:

in water at 14.84; under 750.075 Torr; for 12 h;Sonication;Inert atmosphere;Irradiation;Electrolysis;

Steps:

2.2.1. Photoreforming experiments

General procedure: Kinetic experiments were performed in a Pyrex top-irradiationphoto-reactor connected to a closed gas-circulation system [18].The setup is equipped with facilities for online gas-analysis andliquid-phase sampling. Irradiation is provided by a 300W Xe lampwith a cold mirror 1 (CM 1). A water filter with quartz windowscloses the top of the photo-reactor. The photon flux within the reactor at water level is 8.08 x 1017 s-1 (λ < 390 nm). Typically,75 mg of photocatalyst were ultrasonically dispersed in 100 mLof a 20 mM aqueous reactant solution. The system was deaeratedby four consecutive evacuations and Ar filling cycles. All reactionswere carried out at 288 K and an Ar pressure of 1 bar.

References:

Sanwald, Kai E.;Berto, Tobias F.;Eisenreich, Wolfgang;Gutiérrez, Oliver Y.;Lercher, Johannes A. [Journal of Catalysis,2016,vol. 344,p. 806 - 816]

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