Nitric Acid → Glyoxylic Acid

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Reaction Steps

The reaction is carried out at the most desirable temperature, typically 20° to 70° C. If the concentration of the nonoxidizing strong acid is sufficient, the nitric acid concentration of the reaction solution can usually be maintained at 0.1 wt. % or lower when 50 wt. % nitric acid is gradually added (dropwise) to an aqueous solution of glyoxal. The total amount of nitric acid added can be a slight excess in relation to the theoretical amount (2/3 mole of nitric acid per mole of glyoxal). For example, 0.7 to 0.8 moles of nitric acid per one mole of glyoxal can be employed. When nitric acid is used in an excess amount, the nitric acid concentration of the reaction solution is increased slightly to about 0.5 wt. % at the end of the nitric acid addition, but the nitric acid concentration solution does not exceed 1 wt. %. The nitric acid concentration continues to decrease further after completion of the addition of nitric acid and usually reaches 0.005 to 0.03 wt. % in about one hour. Therefore, an aqueous solution of glyoxylic acid having a residual nitric acid concentration of 0.01 wt. % or below can be obtained without purification. In conventional nitric acid oxidation processes, the conversion of glyoxal is scarcely increased merely by adding nitric acid at about 40° C., even when the reaction is promoted by adding about 0.1 mole of sulfuric acid or hydrochloric acid, so that an aging step has generally been carried out by heating the reaction solution to about 80° C. after completion of the nitric acid addition. In this invention, by contrast, aging by heating is not necessary.

Provenance & Evidence