Preparation method for acetone peroxide dimer
A technology of acetone peroxide dimer and hydrogen peroxide, which is applied in the field of preparation of acetone peroxide dimer, can solve problems such as dimer instability, and achieve the effects of high product purity, high yield and simple method
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Embodiment 1
[0021] Cool acetone, dichloromethane and hydrogen peroxide to -2°C respectively, add 24.36g of acetone (0.42mol) and 100g of dichloromethane into a 500ml flask and mix well, then add 10ml of sulfuric acid containing 3% methanesulfonic acid Mix the solution, the temperature is -2°C; then add 0.44mol hydrogen peroxide dropwise, the dropping rate is controlled every 35 drops, the addition is completed in about 20 minutes, and stirred for about 30 minutes. Cool to -20°C and let stand for 60h. Transfer the mixed solution to a separatory funnel, vibrate to separate the liquid, and collect the organic phase. Slowly add 12ml of methanesulfonic acid to the collected organic phase, drop the temperature to -5°C after the addition, and let it stand at low temperature for 36 hours, then add 200ml of 2°C water to the mixture, stir gently to suspend it, and use a Bush funnel Suction filtration; wash with 300ml of water at 2°C each time until the pH value is 6.8 to 7.1; after fully draining,...
Embodiment 2
[0025] Add 12.18g of acetone (0.21mol) and 60g of dichloromethane to the 500ml flask and mix evenly, then add 5ml of hydrochloric acid mixed solution containing 3% methanesulfonic acid, and the temperature of the reaction solution is at -2°C. While stirring, add 0.22mol hydrogen peroxide drop by drop, the dropping rate is controlled at 40-45 drops per minute, the addition is completed in about 15 minutes, and the stirring is about 30 minutes. Cool to -20°C and let stand for 36h. Transfer the mixed solution to a separatory funnel, vibrate to separate the liquid, and collect the organic phase. Slowly add 5ml of benzenesulfonic acid to the collected organic phase dropwise, after the addition, cool down to -5°C, and after standing at low temperature for 28 hours, add 80ml of water at 2°C to the mixture, and filter with suction; wash with 150ml of water each time until pH The value is up to 6.9; after being drained, it is naturally dried in the shade to obtain 13.47 g of acetone p...
Embodiment 3
[0028] Add 60g of acetone (1.034mol) and 200g of dichloromethane to the 1000ml flask and mix evenly, then add 20ml of acetic acid mixed solution containing 3% methanesulfonic acid, and the temperature of the reaction solution is at -2°C. While stirring, add 1.12mol hydrogen peroxide drop by drop, the dropping speed is controlled to be 40-50 drops per minute, and the dropping is completed within 60 minutes, and stirred for 30 minutes. At -20°C, let stand for 55h. Transfer the mixed solution to a separatory funnel, vibrate to separate the liquid, and collect the organic phase. Transfer the collected organic phase to a 500ml beaker, slowly add 20ml methanesulfonic acid and 5ml propylsulfonic acid dropwise into the beaker, seal the mouth of the beaker with plastic wrap after the addition, lower the temperature to -5°C, and let it stand for 28h Take out the beaker, unseal it, add 220ml of water at 2°C to the reactant to suspend the product, and filter it with suction; wash with wa...
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