Preparation method and application of a tetraaminoiron ligand-bonded cyclodextrin catalyst
A technology of tetraamino and cyclodextrin, applied in the direction of organic compound/hydride/coordination complex catalysts, chemical instruments and methods, physical/chemical process catalysts, etc. impact and other issues, to achieve good economic and environmental benefits, improve stability, and low input costs
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Embodiment 1
[0025] Weigh 3.0 g of tetraaminomacrocyclic ligand and add it into a 250 mL three-neck flask, add 40 mL of chlorosulfonic acid and 2.0 mL of thionyl chloride, react at 60°C-70°C for 8 hours, add ice water and stir for 1 hour, filter, and use Wash with ice water and dry to obtain the sulfonyl chloride-substituted tetraaminomacrocyclic ligand.
[0026] Weigh 2.7g of the sulfonyl chloride-substituted tetraaminomacrocyclic ligand, add it to a 500mL three-neck flask filled with 100mL of dry tetrahydrofuran solution, add 10mL of n-butyl lithium in n-hexane solution (2.5mol / L), and react at 60°C 20min. After completion of the reaction, add 1.08g of anhydrous FeCl in the above reaction solution 3 , heated at 60°C for 4 h, the solid was collected by filtration, washed with 10 mL of tetrahydrofuran and diethyl ether, and dried to obtain the sulfonyl chloride-substituted tetraaminoiron ligand.
[0027] Add 75mL of distilled water to a 500mL three-necked flask and add 6.0g of β-cyclodex...
Embodiment 2
[0031] Prepare an aqueous solution of organic pollutants with a concentration of 100 μg / L, adjust pH=8.0, take 20 mL and add it to a 50 mL Erlenmeyer flask, add tetraaminoiron ligand-bonded cyclodextrin catalyst and hydrogen peroxide, so that the catalyst, oxidant and The molar concentration ratio of pollutants is 1:100:100. The reaction was oscillated in a constant temperature shaking box at 25°C (rotating speed 200r / min), and samples were taken at 0, 2, 4, 8, 15, and 30 min, and the samples were analyzed by HPLC-MS / MS. Tetraamino iron ligand catalyst / H 2 o 2 The degradation rate of the system to carbamide, acetochlor, metolachlor, isoprocarb and malathion can reach more than 99% within 2 minutes. Tetraamino iron ligand bonded cyclodextrin catalyst / H 2 o 2 The first-order degradation reaction rate of the system to acetamiprid, sulfamethoxazole, sulfathiazole, sulfamethazine, norfloxacin, and thiabendazole is 0.035-0.049min -1 , is 1.3-2.2 times of the degradation rate of...
Embodiment 3
[0033] Prepare a sodium dihydrogen phosphate solution with a concentration of 0.2mol / L, take 5mL and add it to a 15mL centrifuge tube, add a quantitative tetraaminoiron ligand-bonded cyclodextrin catalyst to make the concentration 0.25mmol / L (112.5mg / L) , quickly mixed and transferred to a quartz cuvette, and measured the absorbance at a wavelength of 365nm with a UV spectrophotometer every 120s. The hydrolytic stability of the tetraaminoiron ligand-bonded cyclodextrin catalyst prepared in Example 1 was investigated according to the change of absorbance. The first-order hydrolysis reaction rate of tetraaminoiron ligand-bonded cyclodextrin catalyst is 4.4×10 -5 the s -1 , while the hydrolysis reaction rate of the tetraaminoiron ligand catalyst alone and the hydrolysis reaction rate of the tetraaminoiron ligand / cyclodextrin mixed system were 3.6×10 - 3 the s -1 and 8.0×10 -4 the s -1 , are respectively 82 times and 20 times of the hydrolysis reaction rate of tetraaminoiron...
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