A method for synthesizing azelaic acid through combined oxidation of hydrogen peroxide and potassium permanganate
A technology of potassium permanganate and hydrogen peroxide, which is applied to chemical instruments and methods, separation/purification of carboxylic acid compounds, oxidation to prepare carboxylic acids, etc., can solve problems such as troublesome post-processing, short reaction time, and ozone explosion. Achieve the effects of saving time, speeding up the reaction speed and increasing the oxidation capacity
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Embodiment 1
[0012] In a 500mL four-neck flask equipped with an electromagnetic stirrer, a thermometer, and a condenser, add 50 grams of oleic acid, 5 grams of phosphotungstic acid catalyst, and 3 grams of benzyltriethylammonium chloride, and the flow rate of oxygen is 15g. / L. Quickly stir and heat to 75°C, add 2 grams of potassium permanganate, add 200ml of hydrogen peroxide with a mass concentration of 15%, and react for 5 hours. After the reaction, put the mixed solution in a separatory funnel for separation. The lower part of the water layer and the upper part of the oil layer are easy to separate. Refrigerate and crystallize the separated water phase at 3°C; wash the manganese dioxide with 300ml of boiling water three times, heat and concentrate the obtained liquid at 100°C to 50mL, and refrigerate at 0-5°C for crystallization, white powder is precipitated, and the two parts The liquid is suction filtered and dried to obtain azelaic acid, and the calculated yield is about 90.01%. T...
Embodiment 2
[0014] In a 500mL four-neck flask equipped with an electromagnetic stirrer, a thermometer, and a condenser tube, add 50 grams of oleic acid, 5 grams of phosphotungstic acid catalyst, and 3 grams of benzyltriethylammonium chloride. 20g / L. Quickly stir and heat to 95°C, add 2 grams of potassium permanganate, add 200ml of hydrogen peroxide with a mass concentration of 30% in batches, and react for 6 hours. Manganese is in the lower part of the water layer, and the oil layer is on the top, which is easy to separate. Refrigerate and crystallize the separated water phase at 0~5°C; wash manganese dioxide three times with 300ml of boiling water, heat and concentrate the obtained liquid at 100°C to 50mL, refrigerate and crystallize at 0~5°C, white powder precipitates, and The two parts of the liquid were suction filtered and dried to obtain azelaic acid, and the calculated yield was about 99.01%. The melting point is 105.5-107.0°C.
Embodiment 3
[0016] In a 500mL four-neck flask equipped with an electromagnetic stirrer, a thermometer, and a condenser tube, add 50 grams of oleic acid, 5 grams of phosphotungstic acid catalyst, and 3 grams of benzyltriethylammonium chloride. 5g / L. Quickly stir and heat to 60°C, add 2 grams of potassium permanganate, add 200ml of hydrogen peroxide with a mass concentration of 5% in batches, and react for 1 hour. Manganese is in the lower part of the water layer, and the oil layer is on the top, which is easy to separate. Refrigerate and crystallize the separated water phase at 0~5°C; wash manganese dioxide three times with 300ml of boiling water, heat and concentrate the obtained liquid at 100°C to 50mL, refrigerate and crystallize at 0~5°C, white powder precipitates, and The two parts of the liquid were suction filtered and dried to obtain azelaic acid, and the calculated yield was about 69.01%. The melting point is 104.5-106.0°C.
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