Phosphonium salt, catalyst for polymerization of alkylene oxide compound, and process for production of poly(alkylene oxide)
A polymerization catalyst, polyalkylene oxide technology, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, phosphorus organic compound, etc., can solve the impact of polyurethane physical properties, complicated procedures, and poor polymerization activity Sufficient and other issues to achieve the effect of simple manufacturing
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Embodiment 1
[0118] [Synthesis of Tris[tris(dimethylamino)phosphoranylideneamino]phosphonium methoxide (a)]
[0119]
[0120] Under a nitrogen atmosphere, weigh 25.5g (185.6mmol) of phosphorus trichloride in a 1L flask, and dissolve it in 360mL of benzene. At 20°C, a 60 mL benzene solution of 165.5 g (928.9 mmol) of iminotris(dimethylamino)phosphorane was slowly dropped thereinto, followed by allowing to react at 20°C for 2 hours. The iminotris(dimethylamino)phosphorane used is 5.0 mole times that of phosphorus trichloride. After the reaction, the generated precipitate was filtered out, washed with benzene, and combined with the filtrate. Next, the product was extracted from the filtrate into the aqueous phase with 90 mL of water, and then extracted from the aqueous into the organic phase with 600 mL of dichloromethane. After washing the organic phase with water, the solvent was concentrated to dryness to obtain 109.7 g of a white solid.
[0121] As described below, from the white so...
Embodiment 2
[0134] [Synthesis of tris[tris(di-n-propylamino)phosphoranylideneamino]phosphonium methanolate (c)]
[0135]
[0136] Under a nitrogen atmosphere, 253 mg (1.84 mmol) of phosphorus trichloride was weighed in a 100 mL flask and dissolved in 25 mL of pentane. A liquid obtained by dissolving 4.46 g (12.9 mmol) of iminotris(di-n-propylamino)phosphorane in 25 mL of pentane was slowly added dropwise thereto at 0°C. Then, it was made to react at 50 degreeC for 6 hours, and the produced|generated precipitate was filtered off. The dried white solid was 3.42 g. When the white solid was subjected to mass spectrometry, it was observed that tris[tris(di-n-propylamino)phosphoranylideneamino]phosphonium chloride was substituted with the methoxide anion of the phosphonium salt (c) by the chloride anion, and tris[tris(di-n-propylamino)phosphoranylideneamino]phosphonium chloride as Molecular ion peaks corresponding to the molecular weights of the cation moieties of aminotris(di-n-propylamin...
Embodiment 3
[0141] [Synthesis of tris[tris(di-n-hexylamino)phosphoranylideneamino]phosphonium methanolate (d)]
[0142]
[0143] Except changing the usage amount of phosphorus trichloride to 367mg (2.67mmol) in Example 2, using 8.01g (13.4mmol) iminotris(di-n-hexylamino)phosphorane instead of iminotris(di-n-propylamino) ) phosphorane, except that the reaction time was changed to 8 hours, the reaction and post-treatment were carried out in the same manner as in Example 2 to obtain 1.60 g (0.860 mmol) of tris[tris(di-n-hexylamino)phosphoranylideneamino]phosphonium chloride . The yield based on phosphorus trichloride was 32.2%.
[0144] Tris[tris(di-n-hexylamino)phosphoranylideneamino]phosphonium chloride in THF-d 8 with HMPA as the internal standard 31 The chemical shifts of P-NMR were 20.4 ppm and -29.5 ppm, which were assigned to tris[tris(di-n-hexylamino)phosphoranylideneamino]phosphonium cation ([( n Hex 2 N) 3 P=N] 3 PH + ) in P=N in phosphorus atom and PH + phosphorus atom...
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