Phosphonium salt, catalyst for polymerization of alkylene oxide compound, and process for production of poly(alkylene oxide)
A polyalkylene oxide, active hydrogen compound technology, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, phosphorus organic compound, etc., can solve the influence of polyurethane physical properties, complicated procedures, residual amines odor and other problems, 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 methoxide (c)]
[0135]
[0136] Under a nitrogen atmosphere, weigh 253 mg (1.84 mmol) of phosphorus trichloride in a 100 mL flask, and dissolve it in 25 mL of pentane. At 0°C, 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. Thereafter, it was reacted at 50° C. for 6 hours, and the generated precipitate was filtered off. The dried white solid was 3.42 g. Upon mass spectrometry analysis of the white solid, it was observed that tris[tris(di-n-propylamino)phosphoranylideneamino]phosphonium chloride was substituted with the methoxide anion of the phosphonium salt (c) as the chloride anion, and as the A molecular ion peak corresponding to the molecular weight of the cationic portion of aminotris(di-n-propylamino)phosphorane and hydrogen chloride salt.
[0137] Next, the aminotris(di-n-propylamino...
Embodiment 3
[0141] [Synthesis of Tris[tris(di-n-hexylamino)phosphoranylideneamino]phosphonium methoxide (d)]
[0142]
[0143] In addition to changing the 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, change the reaction time to outside 8 hours, carry out reaction and aftertreatment similarly with embodiment 2, obtain 1.60g (0.860mmol) three [three (di-n-hexyl amino) phosphoranylidene amino] phosphonium chloride . The yield based on phosphorus trichloride was 32.2%.
[0144] Tris[tris(di-n-hexylamino)phosphoranylideneamino]phosphonium chloride in THF-d 8 HMPA was used as internal standard in 31 The chemical shifts of P-NMR are 20.4ppm and -29.5ppm, which belong to three [three (di-n-hexylamino) phosphoranylidene amino] phosphonium cations ([( n Hex 2 N) 3 P=N] 3 pH + ) in P=N in the phosphorus atom and PH + phosphorus atoms in the . In additi...
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