Preparation method of polyquaternary ammonium salt, product obtained with method, and application thereof
A polyquaternary ammonium salt, reaction temperature technology, applied in the direction of botanical equipment and methods, applications, chemicals for biological control, etc., to achieve the effects of easy biodegradation, mild reaction conditions, and high yield
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Embodiment 1
[0027] Polyquaternium salts were prepared using tris(2-chloroethyl)phosphate and N,N,N',N'-tetramethylethylenediamine.
[0028] 28.6g (0.1mol) tris (2-chloroethyl) phosphate and 17.4g (0.15mol) N, N, N', N'-tetramethylethylenediamine were added to a 250ml reaction flask, and 100g of Water and ethanol, under nitrogen protection, heated up to 80°C for 30 h, cooled, and removed ethanol under reduced pressure. The obtained compound was recrystallized with ethanol-ethyl acetate mixed solvent to obtain 38.4 g of solid (yield 83.4%).
[0029] Product's 13 The results of C NMR analysis show that the N-CH with a chemical shift of 45.22 in the raw material N, N, N', N'-tetramethylethylenediamine 3 The peak disappears and a quaternary ammonium N with a chemical shift of 52.38 is generated + -CH 3 Peak, raw material tris (2-chloroethyl) phosphate chemical shift is that the C-Cl peak of 42.34 disappears, and generation chemical shift is the quaternary ammonium N of 64.37 + -CH 2 -peak...
Embodiment 2
[0031] Tris(3-chloropropyl)phosphine oxide, hexamethyltriethylenetetramine
[0032] Add 27.9g (0.1mol) tris(3-chloropropyl)phosphine oxide and 17.3g (0.075mol) hexamethyltriethylenetetramine into a 250ml reaction flask, add 100g butanol, protect with nitrogen, and heat up to 90°C After reacting for 30 h, cooling, butanol was removed under reduced pressure, and the obtained compound was recrystallized with ethanol-ethyl acetate mixed solvent to obtain 37.8 g of solid (yield 82.7%).
[0033] Product's 13 The results of C NMR analysis show that the N-CH with chemical shifts of 42.51 and 44.71 3 The peak disappears, and the quaternary ammonium N with chemical shifts of 48.99 and 52.38 is generated + -CH 3 Peak, raw material three (3-chloropropyl) phosphine oxide chemical shift is that the C-Cl peak of 43.12 disappears, and generation chemical shift is the quaternary ammonium N of 62.29 + -CH 2 -peak.
Embodiment 3
[0035] Tris(3-chloro-2-hydroxypropyl)phosphine oxide, pentamethyldiethylenetriamine
[0036] 32.8g (0.1mol) tris(3-chloro-2-hydroxypropyl) phosphine oxide, and 17.3g (0.1mol) pentamethyldiethylenetriamine were added to a 250ml reaction flask, 100g absolute ethanol was added, nitrogen Protect, raise the temperature to 80°C for 250h, cool, remove ethanol under reduced pressure, and recrystallize the obtained compound with ethanol-ethyl acetate mixed solvent to obtain 43.7g of solid (yield: 87.2%).
[0037] Product's 13 The results of C NMR analysis show that the N-CH 3 The peak disappears, and the quaternary ammonium N with chemical shifts of 48.42 and 52.66 is generated + -CH 3 Peak, raw material three (3-chloro-2-hydroxypropyl) phosphine oxide chemical shift is that the C-Cl peak of 46.88 disappears, and generation chemical shift is the quaternary ammonium N of 65.31 + -CH 2 -peak.
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