Polymer containing phosphonic acid group and salt thereof, preparation method and application thereof
A technology of phosphonate group and polymer is applied in the synthesis of phosphonylated polyarylene ether polymer and its preparation, and the field of new polymer materials, which can solve the problem of increasing the cost of water purification treatment, easy deformation and weak resistance. power and other issues
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Embodiment 1
[0053] Preparation of diethyl 3-cyano-2,4-difluorophenylphosphonate:
[0054] (1) Preparation of 3-bromo-2,6-difluorobenzonitrile:
[0055]
[0056] Take a 2 L four-neck flask, add 600 mL of 60% sulfuric acid, add 139.0 g (1.0 mol) of 2,6-difluorobenzonitrile under electric stirring, and 2 Under protection, control the reaction temperature below 35°C, add 250.5 g of KBrO in 10 batches 3 (1.5 mol), monitored by TLC, reacted for 5-6 days, stopped the reaction after the raw material point disappeared, prepared 800 mL of 20% ice-salt solution, and poured the reaction solution into ice-salt water. After the product settles, quickly carry out suction filtration to obtain an orange crude product, which is washed with CCl 4 Dissolve the crude product with 5% NaHSO 3 solution, saturated Na 2 CO 3 Wash the solution and water until the solution is neutral, dry it with anhydrous sodium sulfate, filter the solution, and steam in a water bath at 60°C to obtain a light yellow liquid,...
Embodiment 2
[0061] Preparation of phosphonate polymer (Ⅲ-1):
[0062]
[0063] (Ⅲ-1)
[0064] Under nitrogen atmosphere, diethyl 3-cyano-2,4-difluorophenylphosphonate (3.85 g, 14.0 mmol), 4,4 · -Dichlorodiphenylsulfone (1.72 g, 6.0 mmol), biphenol (3.72 g, 20.0 mmol), anhydrous potassium carbonate (3.18 g, 23.0 mmol), N,N-dimethylacetamide (DMAc, 56 mL), toluene (28 mL) were mixed and heated to 160°C, water was separated for 4 hours, the toluene was distilled off, the temperature was raised to 180°C, and the reaction was carried out for 36 hours. Slowly pour the reaction solution into 400 mL of deionized water to obtain a white strip polymer, change the water, keep the temperature at 80°C, boil in water three times, each time for 6 hours, dry, and then vacuum dry at 100°C for 24 hours to obtain white fibers The obtained polymer was 7.96 g, the yield was 96%, and the intrinsic viscosity was 0.56 dL / g.
Embodiment 3
[0066] Preparation of phosphonate polymer (Ⅲ-2):
[0067]
[0068] (Ⅲ-2)
[0069] Under nitrogen atmosphere, diethyl 3-cyano-2,4-difluorophenylphosphonate (3.85 g, 14.0 mmol), 4,4 · -Dichlorodiphenylsulfone (1.72 g, 6.0 mmol), bisphenol A (4.57 g, 20.0 mmol), anhydrous potassium carbonate (3.18 g, 23.0 mmol), N,N-dimethylacetamide (DMAc, 56 mL), toluene (28 mL) were mixed and heated to 160°C, water was separated for 4 hours, the toluene was distilled off, the temperature was raised to 180°C, and the reaction was carried out for 36 hours. Slowly pour the reaction solution into 400 mL of deionized water to obtain a white strip polymer, change the water, keep the temperature at 80°C, boil in water three times, each time for 6 hours, dry, and then vacuum dry at 100°C for 24 hours to obtain white fibers The obtained polymer was 8.78 g, the yield was 96%, and the intrinsic viscosity was 0.49 dL / g.
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