A kind of synthetic method of hindered phenolic antioxidant 3114
A synthesis method and technology of hindered phenols, applied in ether preparation, organic chemistry and other directions, can solve the problems of many side reactions, high equipment requirements, environmental pollution, etc., and achieve the effects of less equipment investment, good economy, and safe operation.
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Embodiment 1
[0026] Example 1 Synthesis of intermediate (3.5-di-tert-butylphenol-4-hydroxyl) benzyl methyl ether.
[0027] Add 103g of 2,6-di-tert-butylphenol and 24g of paraformaldehyde into a 1000ml four-neck flask equipped with mechanical stirring, thermometer socket, reflux condensing device, and constant pressure dropping funnel, vacuumize, and replace with nitrogen for more than 3 times , and under nitrogen protection, add catalyst dimethylamine aqueous solution (mass concentration is 33%) 6.8g and 95% methanol aqueous solution 400mL from the constant pressure dropping funnel, heat and reflux under nitrogen protection for 6 hours, steam about 50% after the reaction % methanol, the temperature of the reaction product was lowered to 50°C, and 23.5ml of distilled water was added from the constant pressure dropping funnel. The product was washed with a small amount of methanol and dried to obtain white granular crystals, namely the intermediate (3.5-di-tert-butylphenol-4-hydroxyl) benz...
Embodiment 2
[0035] Example 2 Synthesis method of hindered phenolic antioxidant 3114.
[0036] Add the intermediate (3.5-di-tert-butylphenol-4-hydroxyl) benzyl 110g of methyl ether, 17.2g of isocyanuric acid, 250ml of dimethylformamide, vacuumize, replace with nitrogen more than 3 times, raise the temperature under the protection of nitrogen, start stirring, after all the materials are dissolved, add the catalyst triethylamine from the constant pressure funnel 1g, seal the reaction system, close the nitrogen inlet glass valve, turn on the vacuum pump, feed the 60°C circulating water into the reflux condensing device, the reaction solvent dimethylformamide is continuously refluxed, and the by-product methanol is continuously taken out by the vacuum system and recovered, controlled The degree of vacuum is between -0.05-0.07MP, and the reaction temperature is between 135-140°C. If the degree of vacuum is too high, the reaction solvent will be easily drawn out. React under these conditions ...
Embodiment 3
[0040] Example 3 The synthesis method of hindered phenolic antioxidant 3114.
[0041]Add intermediate (3.5-di-tert-butylphenol-4-hydroxyl) benzyl methyl ether 110g, isocyanuric acid 17.2 g. 250ml of dimethylformamide, 1g of urotropine, evacuated nitrogen for more than 3 times, heated up under the protection of nitrogen, started stirring, after all the materials were dissolved, sealed the reaction system, and closed the nitrogen inlet glass valve, opened Vacuum pump and reflux condensing device are fed with 60°C circulating water, the reaction solvent dimethylformamide is continuously refluxed, and the by-product methanol is continuously taken out and recovered by the vacuum system, the vacuum degree is controlled between -0.05-0.07MP, and the reaction temperature is 135 Between -140°C, if the vacuum is too large, the reaction solvent will be easily drawn out. React under these conditions for 5 hours, quickly cool down to room temperature, add a small amount of 3114 as a see...
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