Photoresponse type polyoxometalate catalyst and application thereof in homogeneous catalysis and heterogeneous recycling
A multi-metal oxygen cluster, homogeneous catalysis technology, applied in chemical recovery, physical/chemical process catalyst, organic compound/hydride/coordination complex catalyst, etc. problem, to achieve the effect of simple operation and a wide range of solvents
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Embodiment 1
[0052] Synthesis of N,N-dimethyldecyl(10-(4'-oxyazobenzene))decylammonium bromide surfactant molecule (S-1), whose structural formula is as follows:
[0053]
[0054] 5.0 g of p-hydroxyazobenzene, 15.2 g of 1,10-dibromodecane, 7.0 g of anhydrous potassium carbonate, catalyst amount of 18-crown-6 and 150 ml of acetone were mixed, stirred and refluxed for 24 hours under nitrogen protection. After the reaction, the reaction solution was naturally cooled to room temperature, and the insoluble solid salt was removed by filtration, and the filtrate was evaporated to dryness under reduced pressure. The resulting liquid crude product was purified by column chromatography using a mixed solvent of petroleum ether / chloroform with a volume ratio of 2:1 as an eluent to obtain 7.6 grams of a yellow solid product, which is 1-bromo-10-(4'-oxyl Azobenzene) decane, the productive rate is 72.4%.
[0055] 2.7 grams of dimethyldecylamine and 5 grams of 1-bromo-10-(4'-oxyazobenzene) decane were...
Embodiment 2
[0057] Synthesis of N,N-dimethylbis(8-(4'-oxyazobenzene))octylammonium bromide surfactant molecule (S-2), whose structural formula is as follows:
[0058]
[0059] Mix 2.0 g of p-hydroxyazobenzene, 5.5 g of 1,8-dibromooctane, 2.8 g of anhydrous potassium carbonate, catalytic amount of 18-crown-6 and 150 ml of acetone, and stir and reflux for 24 hours under nitrogen protection. After the reaction, the reaction solution was naturally cooled to room temperature, and the insoluble solid salt was removed by filtration, and the filtrate was evaporated to dryness under reduced pressure. The resulting liquid crude product was purified by column chromatography using a mixed solvent of petroleum ether / chloroform with a volume ratio of 2:1 as the eluent to obtain 2.3 grams of a yellow solid product, which was 1-bromo-8-(4'-oxyl Azobenzene) octane, the productive rate is 58.2%.
[0060] 2.5 grams of 33% dimethylamine aqueous solution and 1.0 grams of 1-bromo-8-(4'-oxyazobenzene) octan...
Embodiment 3
[0063] Synthesis of N,N-dimethylbis(6-(4'-oxyazobenzene))hexylammonium bromide surfactant molecule (S-3), whose structural formula is as follows:
[0064]
[0065] Mix 5.0 g of p-hydroxyazobenzene, 12.3 g of 1,6-dibromohexane, 7.0 g of anhydrous potassium carbonate, catalytic amount of 18-crown-6 and 150 ml of acetone, and stir and reflux for 24 hours under nitrogen protection. After the reaction, the reaction solution was naturally cooled to room temperature, and the insoluble solid salt was removed by filtration, and the filtrate was evaporated to dryness under reduced pressure. The resulting liquid crude product was purified by column chromatography using a mixed solvent of petroleum ether / chloroform with a volume ratio of 2:1 as the eluent to obtain 5.5 grams of a yellow solid product, which was 1-bromo-6-(4'-oxyl Azobenzene) hexane, the productive rate is 59.3%.
[0066] 5.3 grams of 33% dimethylamine aqueous solution and 2.0 grams of 1-bromo-6-(4'-oxyazobenzene) hexa...
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