Process for alkaline hydrolysis of carboxylic acid derivatives to carboxylic acids
A carboxylic acid derivative, alkaline technology, applied in the preparation of carboxylic acid anhydride, fatty acid production, preparation of carboxylate/lactone, etc., can solve problems such as high cost elements and cost increase
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Embodiment 2
[0035] Embodiment 2: Alkaline Hydrolysis Carboxylate
[0036] In a reaction vessel with a stirrer and a reflux cooler, 100 grams of ethyl 2-methylbutyrate was mixed into 200 grams of red mud, wherein the residual water content of the red mud exceeded 10%. The mixture can optionally be diluted with water or an inert solvent in order to ensure adequate mixing without problems. When liquid carboxylic acid esters are used, they can basically also be added in excess, so that they themselves function as solvents. The mixture was stirred with stirring at room temperature for about 2 hours, wherein ethyl 2-methylbutyrate was saponified to 2-methylbutyric acid and ethanol. Towards the end of the reaction, the reaction temperature can optionally be increased and the mixture is boiled at reflux in order to ensure as complete a conversion as possible. After cooling, the mixture was filtered and the liquid phase was extracted several times with hexane. The combined organic phases were t...
Embodiment 3
[0037] Embodiment 3: basic hydrolysis carboxylic acid chloride
[0038] 20 grams of pyridine was mixed into 5 grams of red mud in a reaction vessel with reflux cooler, drying tube and dropping funnel. About 2 grams of benzoyl chloride were carefully added dropwise with stirring. After the addition, the mixture was heated on a water bath for 10 minutes. Optionally, it can also be stirred at room temperature for 1 hour. After cooling, ice water was added, and the mixture was filtered through a glass frit, wherein the dealkalized red mud contained in the amorphous filter cake was subsequently washed with ice water. Alternatively, the dealkalized red mud can also be separated from the liquid phase by sedimentation followed by decantation. The filtrate was then acidified with concentrated hydrochloric acid and extracted 3 times with ether. The combined ether phases are washed successively with saturated sodium bicarbonate solution and saturated sodium chloride solution and drie...
Embodiment 4
[0039] Embodiment 4: Alkaline hydrolysis of carboxylic acid anhydride
[0040] In the reaction vessel with reflux cooler, drying tube and dropping funnel, water was mixed in an amount of 20 g of red mud to ensure reliable and thorough mixing. About 5 grams of maleic anhydride was added dropwise with vigorous stirring. After the addition, the mixture was heated on a water bath for 20 minutes and, after cooling, poured into ice water. The dealkalized red mud was sucked through a frit and washed with ice water. The liquid phase is worked up in a known manner to obtain the product maleic acid.
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