Preparation method of acetophenone
A technology of acetophenone and cumene, which is applied in the field of preparation of acetophenone, can solve the problems of expensive reaction cost, high requirements for catalyst and reaction device, and achieve the effects of low reaction cost, environmental friendliness and simple operation
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[0025] The invention provides a kind of preparation method of acetophenone, comprises the following steps:
[0026] 1) Under heating conditions, oxygen is used to oxidize the alkaline solution containing cumene to obtain an oxidation reaction solution;
[0027] 2) adding the ferrous sulfate solution into the oxidation reaction solution to react to obtain acetophenone.
[0028] Above-mentioned preparation method can be represented by following reaction formula:
[0029]
[0030] The inventor speculates that this reaction has experienced the following reaction process:
[0031] In step 1), heating conditions can cause cumene to generate free radical intermediates, which can be further reacted to obtain cumene hydroperoxide after reacting with oxygen;
[0032] In step 2), ferrous sulfate can be used as a reducing agent to reduce cumene hydroperoxide, and the reduction goes through two stages. First, under the action of ferrous sulfate, cumene hydroperoxide removes a molecule...
Embodiment 1
[0051] The preparation method of present embodiment acetophenone comprises the following steps:
[0052] 1) Add cumene (1200g, 10mol) into a 2L autoclave, then add 0.3g of sodium carbonate and 100mL of water, seal and stir;
[0053] 2) Feed nitrogen into the autoclave to 1.0-1.1MPa, then heat to 110°C, feed oxygen, and open the tail gas valve, control the flow of oxygen to 0.25L / min, keep the flow for one hour, adjust the oxygen Flow rate to 0.4L / min, after continuing to react for 5h, stop the reaction to obtain the oxidation reaction solution;
[0054] 3) FeSO 4 ·7H 2 O (3336g, 12mol) was dissolved in 33.36kg of water to obtain a ferrous sulfate solution. The controlled temperature was 10-15°C and the ferrous sulfate solution was added to the oxidation reaction solution at a rate of 400g / min. After the addition was complete, continue Insulation reaction 10min;
[0055] 4) After the heat preservation is completed, the reaction solution is separated, and the organic phase i...
Embodiment 2
[0063] The preparation method of present embodiment acetophenone comprises the following steps:
[0064] 1) Add cumene (1200g, 10mol) into a 2L autoclave, then add 0.5g of sodium carbonate and 100mL of water, seal and stir;
[0065] 2) Feed nitrogen into the autoclave to 1.0-1.1MPa, then heat to 110°C, feed oxygen, and open the tail gas valve, control the flow of oxygen to 0.25L / min, keep the flow for one hour, adjust the oxygen Flow rate to 0.4L / min, after continuing to react for 5h, stop the reaction to obtain the oxidation reaction liquid;
[0066] 3) FeSO 4 ·7H 2 O (3336g, 12mol) was dissolved in 33.36kg of water to obtain a ferrous sulfate solution. The controlled temperature was 10-15°C and the ferrous sulfate solution was added to the oxidation reaction solution at a rate of 400g / min. After the addition was complete, continue Insulation reaction 10min;
[0067] 4) After the heat preservation is completed, the reaction liquid is separated, and the organic phase is an...
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