Ionic liquid containing phosphonium ion and method for producing same
A technology of ionic liquids and cations, applied in the manufacture of final products, chemical instruments and methods, sustainable manufacturing/processing, etc., can solve problems such as low viscosity, obstacles in the application of electrolytes, electrolytes or additives, and high conductivity
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment
[0044] (a) the preparation of three (dimethylamino) methoxyphosphonium methyl sulfates
[0045] Use a two-necked eggplant-shaped flask equipped with a reflux cooling tube, a dropping funnel, and a magnetic stirrer at room temperature under N 2 Under an atmosphere, 1.4 g (11.2 mmol) of dimethyl sulfate was added dropwise to 2.0 g (11.2 mmol) of hexamethylphosphate triamide, and stirred at room temperature for 15 hours to obtain a white solid salt. Wash thoroughly with diethyl ether, and vacuum-dry at 50° C. for 5 hours to obtain tris(dimethylamino)methoxyphosphonium methyl sulfate with a yield of 74%.
[0046] Compound identification was carried out using a nuclear magnetic resonance analyzer (BRUKER Ultra Shield 300 NMR Spectrometer manufactured by BRUKER). Spectral data are shown below.
[0047] 1 H-NMR (300MHz, solvent: acetone-d6, standard substance: tetramethylsilane)
[0048] δ4.06(d,3H)
[0049] 3.47(s, 3H)
[0050] 2.90 (d, 18H)
[0051] The structural formula is...
Embodiment 2
[0066] (c) Preparation of three (dimethylamino) ethoxyphosphonium ethyl sulfate
[0067] Use a two-necked eggplant-shaped flask equipped with a reflux cooling tube, a dropping funnel, and a magnetic stirrer at room temperature under N 2 Under an atmosphere, 2.1 g (13.4 mmol) of diethyl sulfate was added dropwise to 2.0 g (11.2 mmol) of hexamethylphosphoric acid triamide, and stirred at 20° C. for 5 days to obtain a white solid salt. Wash thoroughly with diethyl ether, and vacuum-dry at 50° C. for 5 hours to obtain ethyl tris(dimethylamino)ethoxyphosphonium sulfate with a yield of 87%.
[0068] Compound identification was carried out using a nuclear magnetic resonance analyzer (BRUKER Ultra Shield 300 NMR Spectrometer manufactured by BRUKER). Spectral data are shown below.
[0069] 1 H-NMR (300MHz, solvent: acetone-d6, standard substance: tetramethylsilane)
[0070] δ4.47 4.38 (m, 2H)
[0071] 3.86(q,2H)
[0072] 2.90 (d, 18H)
[0073] 1.45(t,3H)
[0074] 1.13(t,3H)
...
Embodiment 3
[0090] (e) Preparation of three (dimethylamino) butoxyphosphonium butyl sulfates
[0091] Use a two-necked eggplant-shaped flask equipped with a reflux cooling tube, a dropping funnel, and a magnetic stirrer at room temperature under N 2 Under the atmosphere, 70.4 g (335 mmol) of dibutyl sulfate was added dropwise to 50.0 g (279 mmol) of hexamethylphosphoric triamide, and stirred at 30° C. for 7 days to obtain a white solid salt. Wash thoroughly with diethyl ether, and vacuum-dry at 50° C. for 5 hours to obtain tris(dimethylamino)butoxyphosphonium butyl sulfate with a yield of 93%.
[0092] Compound identification was carried out using a nuclear magnetic resonance analyzer (BRUKER Ultra Shield 300 NMR Spectrometer manufactured by BRUKER). Spectral data are shown below.
[0093] 1 H-NMR (300MHz, solvent: acetone-d6, standard substance: tetramethylsilane)
[0094] δ4.38(q,2H)
[0095] 3.82(t,2H)
[0096] 2.90 (d, 18H)
[0097] 1.80-1.73(m, 2H)
[0098] 1.55-1.30(m, 6H) ...
PUM
| Property | Measurement | Unit |
|---|---|---|
| melting point | aaaaa | aaaaa |
| melting point | aaaaa | aaaaa |
| melting point | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More 