Production method of high-purity dioctyl diphenylamine antioxidant
A technology of dioctyldiphenylamine and its production method, which is applied in the direction of additives, amino compound purification/separation, condensation/addition reaction to prepare amino compounds, etc., to achieve the effects of low temperature, low corrosion, and mild reaction conditions
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Embodiment 1
[0037] 600g of nitromethane was added into a four-necked flask with a thermometer, a stirrer, a reflux condenser and a cold bath, and N 2 , under the condition of room temperature and temperature control, slowly add 300g of anhydrous aluminum trichloride while stirring, stir until completely dissolved, obtain 900g of anhydrous aluminum trichloride complex catalyst, pour it into a brown narrow mouth bottle, Cap the bottle and set aside.
[0038] Add 169g of diphenylamine and 50.7g of aluminum trichloride complex catalyst into a 2L stainless steel reaction kettle, cover the lid of the kettle, install the thermocouple and stir, then turn on the heating switch, raise the temperature to 100°C, stir for 1 hour, and then once 784g of diisobutene was pumped in, and the reaction was continued at 100°C for 8 hours with constant stirring. Then cool down to room temperature, pour the material into a separatory funnel, let stand to separate layers, and separate and remove the lower cataly...
Embodiment 2
[0040] Add 169g of diphenylamine and 50.7g of the aluminum trichloride complex catalyst prepared in Example 1 into a 2L stainless steel reaction kettle, cover the gland, install the thermocouple, stir, turn on the heating switch, and raise the temperature to 100°C , stirred for 1 h, and then pumped 784 g of diisobutylene in one go, and continued to react at a constant temperature of 100 ° C for 8 h. Then cool down to room temperature, pour the material into a separatory funnel, let stand to separate layers, and separate and remove the lower catalyst layer. The crude product in the upper layer was washed and separated in a separatory funnel according to the crude product:water mass ratio of 100:20, and washed with hot water. The washing temperature was controlled at 60°C and washed 3 times with water. At 80°C and -0.06~-0.08MPa, the crude product after washing and separation was subjected to vacuum distillation in a three-neck flask for 2 hours. The gas-phase condensed componen...
Embodiment 3
[0042] Add 169g of diphenylamine and 50.7g of the aluminum trichloride complex catalyst prepared in Example 1 into a 2L stainless steel reaction kettle, cover the gland, install the thermocouple, stir, turn on the heating switch, and raise the temperature to 100°C , stirred for 1 h, and then pumped 784 g of diisobutylene in one go, and continued to react at a constant temperature of 100 ° C for 8 h. Then cool down to room temperature, pour the material into a separatory funnel, let stand to separate layers, and separate and remove the lower catalyst layer. Put the crude product in the upper layer into a 2L stainless steel reaction kettle, add 10g of activated clay, cover the gland, install the thermocouple, stir, turn on the heating switch, raise the temperature to 110°C, and stir for 1h to decolorize. Then cool down to 80°C, heat filter the decolorized crude product, wash and separate the filtrate in a separatory funnel according to the mass ratio of filtrate:water 100:20, wa...
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