Preparation method of alkyloxy azobenzene photosensitive foam control agent
A technology of alkyloxyazobenzene and foam control agent is applied in the field of preparation of photosensitive foam control agent, which can solve the problems of foam waste, pollution and the like, and achieves the effect of solving processing problems and improving uniformity
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Embodiment 1
[0018] (1) Take 14.00wt% p-nitrophenol, 71.00wt% potassium hydroxide and 15.00wt% water in a three-necked flask, heat up to 120°C, keep the temperature for 1h, slowly heat to 200°C, and keep the violent reaction constant until no more Cool to room temperature after the bubbles are generated, dissolve the product in water, then neutralize it with concentrated hydrochloric acid to pH 3, extract with ether, distill off the ether under reduced pressure, and then recrystallize to prepare 4,4'-dihydroxyazobenzene;
[0019] (2) Add 1.20wt% 4,4'-dihydroxyazobenzene, 1.20wt% anhydrous potassium carbonate and 0.83wt% potassium iodide into a three-necked flask, stir and heat up to 80°C, react for 30min, and add 2.00wt% bromine Dodecane was added dropwise to 94.77wt% N,N-dimethylformamide complex solvent, slowly added dropwise into a three-necked flask, reacted at 80°C for 8 hours, cooled to room temperature, and evaporated under reduced pressure to remove N,N-dimethylformamide Methyl for...
Embodiment 2
[0023] (1) Take 18.00wt% p-nitrophenol, 62.00wt% potassium hydroxide and 20.00wt% water in a three-necked flask, heat up to 120°C, keep the temperature for 1h, slowly heat to 200°C, and violently react until no more Cool to room temperature after the bubbles are generated, dissolve the product in water, then neutralize it with concentrated hydrochloric acid to pH 3, extract with ether, distill off the ether under reduced pressure, and then recrystallize to prepare 4,4'-dihydroxyazobenzene;
[0024] (2) Add 1.00wt% 4,4'-dihydroxyazobenzene, 1.00wt% anhydrous potassium carbonate and 0.10wt% potassium iodide into a three-necked flask, stir and heat up to 80°C, react for 30min, and add 1.60wt% bromine Add octane dropwise to 96.30wt% N,N-dimethylformamide complex solvent, slowly add it dropwise into a three-necked flask, react at 80°C for 8h, cool to room temperature, and distill off N,N-dimethylformamide under reduced pressure dichloromethane and water, take the organic layer, dis...
Embodiment 3
[0028] (1) Take 12.00wt% p-nitrophenol, 73.00wt% potassium hydroxide and 15.00wt% water in a three-necked flask, heat up to 120°C, keep the temperature for 1h, slowly heat to 200°C, and keep the violent reaction constant until no more Cool to room temperature after the bubbles are generated, dissolve the product in water, then neutralize it with concentrated hydrochloric acid to pH 3, extract with ether, distill off the ether under reduced pressure, and then recrystallize to prepare 4,4'-dihydroxyazobenzene;
[0029] (2) Add 1.40wt% 4,4'-dihydroxyazobenzene, 1.40wt% anhydrous potassium carbonate and 1.00wt% potassium iodide into a three-necked flask, stir and heat up to 80°C, react for 30min, and add 2.33wt% bromine Butane was added dropwise to 93.87wt% N,N-dimethylformamide complex solvent, slowly added dropwise into a three-necked flask, reacted at 80°C for 8h, cooled to room temperature, and N,N-dimethylformamide was distilled off under reduced pressure. dichloromethane and...
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