Novel ion-exchange material, its preparation and application
An ion exchange material and a new technology, applied in the field of preparation of coordination polymer functional materials, can solve the problems of change, difficult ion exchange process, and difficult post-processing, and achieve high yield, short reaction time, and post-processing convenient effect
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Embodiment 1
[0028] Preparation and Discussion of Bispiperazine Bridged Organic Ligand L Containing Oxadiazole Ring
[0029] 1. Synthesis experiment and post-processing:
[0030] 18.6 g of piperazine-2-carboxylic acid (0.15 mol) and 12.8 g of hydrazine hydrochloride (0.08 mol) were placed in a three-necked flask and stirred and mixed, and then 50 mL of phosphoric acid (85%) was added. Subsequently, 20.1 g of phosphorus pentoxide (0.48 mol) and 23.0 g of phosphorus oxychloride (0.15 mol) were added successively. The viscous solution was heated to 140°C and stirred vigorously for four hours, then cooled to 17°C. Pour twice distilled water into the obtained mucus until the mucus and water are completely combined, and after dissolving, neutralize with sodium bicarbonate until the pH value of the solution is 7. An orange-yellow precipitate precipitated, was filtered, washed three times with 60 mL of anhydrous ether, and then dried in vacuo. Accurately weighed with an analytical balance, the ...
Embodiment 2
[0039] Preparation and Discussion of Bispiperazine-Bridged Organic Ligand L Containing Oxadiazole Ring
[0040] 1. Synthesis experiment and post-processing:
[0041] 4.65 g of piperazine-2-carboxylic acid (0.0375 mol) and 3.2 g of hydrazine hydrochloride (0.02 mol) were placed in a three-necked flask and stirred and mixed, and then 15 mL of phosphoric acid (85%) was added. Subsequently, 5.03 g of phosphorus pentoxide (0.12 mol) and 5.8 g of phosphorus oxychloride (0.0375 mol) were carefully added in succession. The viscous solution was heated to 140°C and stirred vigorously for four hours, then cooled to 25°C.
[0042] Post-treatment process: Pour twice distilled water into the obtained mucus until the mucus and water are completely fused, dissolve and neutralize with sodium bicarbonate until the pH of the solution is 7. An orange-yellow precipitate precipitated, was filtered, washed three times with 20 mL of anhydrous ether, and then dried in vacuo. Weigh accurately with a...
Embodiment 3
[0045] Preparation, structure and discussion of new ion exchange materials 1-4
[0046] 1. Preparation of new materials:
[0047] New ion exchange material 1 (hereinafter referred to as material 1): AgBF 4 (2mmol, 0.39g) and an equimolar amount of L ligand (2mmol, 0.45g) were dissolved in methanol / chloroform (commercially available analytical grade, volume ratio 1:1, 60mL) organic solvent, stirred for 1 hour, and then the obtained The clear solution was left to stand, and with the volatilization of the solvent, material 1 could be obtained after 4 days. Filter, wash with 40 mL of anhydrous ether, and finally vacuum-dry. Calculated yield: 80%.
[0048] New ion exchange material 2 (hereinafter referred to as material 2): AgAsF at a temperature of 30°C 6 (2mmol, 0.60g) and an equimolar amount of L ligand (2mmol, 0.45g) were dissolved in methanol / chloroform (commercially available analytical grade, volume ratio 1:1, 80mL) organic solvent, stirred for 1 hour, and then the obt...
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