report one,
500g of isooctanol, 258g of potassium hydroxide, 10g of zinc formate were added successively to the 2000ml autoclave, the reaction kettle was replaced with nitrogen for 2 times to discharge the air in the system, and the reaction was carried out at 230 ° C and 2Mpa after sealing, and the reaction was carried out. After 6h, the temperature was kept for 50min, then the temperature was lowered to below 160°C, the pressure in the kettle was reduced to normal pressure, 400ml of distilled water was added, and the mixture was stirred for 30min to obtain 2-Ethylhexanoic Acid potassium aqueous solution.
Transfer the 2-Ethylhexanoic Acid potassium aqueous solution to the flask, slowly add 212 g of 94 wt% formic acid solution under stirring, control the reaction temperature to 60 ° C, react for 30 min, move to a separatory funnel, let stand for 30 min, and separate the water phase by layer and water. The phase is simply concentrated to obtain potassium formate solution (the solution can be directly sold as a commodity or concentrated into a certain concentration such as 74% for sale); the oil phase is washed twice with 60g distilled water to obtain thick 2-Ethylhexanoic Acid, and the unreacted alcohol is removed by distillation under reduced pressure. , 542g of isooctanoic acid finished product was obtained by rectification, the yield in terms of isooctanol was 108.4%, and the molar yield was 97.92%.
report two,
In a 2000ml autoclave, 250g of isooctanol, 172g of caustic soda, 1.6g of zinc acetate were added successively, and then 250g of isooctanol was added. The reaction kettle was filled with nitrogen, and the reaction was carried out at 250°C and 2.8MPa. After condensation, it was discharged to the outside. When no hydrogen was released in the reaction, the reaction was kept under pressure for 40 minutes, cooled to below 120 ° C, and then the pressure in the kettle was reduced to normal pressure, 500 ml of distilled water was added, and stirred for 30 minutes to obtain an aqueous solution of sodium isooctanoate.
Add 350g of distilled water to another flask, slowly add 250g of concentrated sulfuric acid under stirring, keep the temperature in the flask not more than 80°C, slowly pour the reactants in the autoclave into the flask, control the reaction temperature to be 70°C, react for 40min, move to Separation funnel, keep the temperature static for 1 hour, then remove the water phase by layers, and recover the refined sodium sulfate after the water phase treatment; the oil phase is washed twice with distilled water at about 70 °C to obtain crude isooctanoic acid, and the unreacted alcohol is distilled off under reduced pressure. , rectification to obtain 2-Ethylhexanoic Acid finished product, the yield is 105%.
