Polyoxyethylene alkylphenol ether ester cationic gemini surfactant and preparation method thereof
A technology of alkylphenol polyoxyethylene ether and alkylphenol polyoxyethylene chloroacetate, which is applied in the field of preparation of the surfactant, can solve the problems of complex reaction process, difficult product purification, and few varieties, and achieves the preparation method Simple, rich source of raw materials, good emulsifying effect
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Embodiment 1
[0033] Add 11.4 g of nonylphenol polyoxyethylene ether (3), 8.1 g of chloroacetic acid, 0.7 g of anhydrous calcium chloride, and 15 mL of benzene into the reaction flask and stir to raise the temperature to reflux. Heating was stopped after reflux for 5 h, benzene was removed by rotary evaporation, the residual liquid was neutralized to pH = 6~7 with 10% potassium carbonate solution, washed several times with saturated brine, and dried over anhydrous sodium sulfate to obtain 10.312 g of light brown liquid chlorine Acetate nonylphenol polyoxyethylene ether (3) ester, yield 73.7%.
[0034] Tablet, cm -1 ):2966.2,2933.5,2872.2,1760.7,1609.5,1580.9,1511.5,1454.3,1413.4,1380.7,1360.3,1290.8,1249.9,1188.6,1139.6,1070.2,1037.5,959.8,927.1,865.8,829.1,775.9,751.4,730.9, 698.3, 681.9, 567.5.
[0035] 1 3 δ (*10 -6 ): 0.48 ~ 0.88(m, 9H), 1.03 ~ 1.73(m, 8H), 3.65 ~ 3.74(m, 8H), 3.83 ~ 3.86 (t, J = 9.3 Hz, 2H), 4.08~ 4.13(m, 2H), 4.33 ~4.35(m, 2H), 6.82 ~ 6.84(d, J = 8.7 Hz, 2...
Embodiment 2
[0037]Add 10.1 g of octylphenol polyoxyethylene ether (6), 5.0 g of chloroacetic acid, 0.5 g of anhydrous calcium chloride, and 30 mL of benzene into the reaction flask, stir and raise the temperature to reflux. Heating was stopped after reflux for 5 h, benzene was removed by rotary evaporation, the residual liquid was neutralized to pH = 6~7 with 10% potassium carbonate solution, washed several times with saturated brine, and dried over anhydrous sodium sulfate to obtain 7.398 g of light brown liquid chlorine Acetate octylphenol polyoxyethylene ether (6) ester, yield 67.8%.
[0038] Tablet, cm -1 ):3038.6, 2957.7, 2923.4, 2871.9, 1758.5, 1609.6, 1580.8, 1512.2, 1458.8, 1413.1, 1377.6, 1351.1, 1293.9, 1249.9, 1186.9, 1127.5, 1039.8, 951.2, 830.6, 782.0, 731.0, 681.9, 568.3。
[0039] 1 3 δ (*10 -6 ): 0.48 ~ 0.88(m, 9H), 1.06 ~ 1.73(m, 8H), 3.48 ~ 3.75(m, 20H), 3.84 ~ 3.86(t, J = 9.6 Hz, 2H), 4.06 ~ 4.12(m, 2H), 4.33~4.35(s, 2H), 6.82 ~ 6.84(d, J = 8.7 Hz, 2H), 7.13 ~...
Embodiment 3
[0041] Add 9.7 g of octylphenol ethoxylate (10), 3.6 g of chloroacetic acid, 0.5 g of anhydrous calcium chloride, and 15 mL of benzene into the reaction flask, stir and raise the temperature to reflux. Heating was stopped after reflux for 6 h, benzene was removed by rotary evaporation, the residual liquid was neutralized to pH = 6~7 with 10% potassium carbonate solution, washed several times with saturated brine, and dried over anhydrous sodium sulfate to obtain 9.464 g of light yellow liquid Octylphenol polyoxyethylene ether (10) chloroacetate, yield 87%.
[0042] Tablet, cm -1 ): 2953.9, 292994, 2872.2, 1748.5, 1605.4, 1578.8, 1511.5, 1454.3, 1417.5, 1380.7, 1348.0, 1290.81249.9, 1188.9, 947.6, 788.2, 730.9, 575.7.
[0043] 1 3 δ (*10 -6 ): 0.48 ~ 0.88(m, 9H), 1.06 ~ 1.60(m, 8H), 3.62 ~ 3.74(m, 24H), 3.84 ~ 3.86(t, J = 9.6 Hz, 2H), 4.10 ~ 4.11(m, 2H), 4.33~4.35(m, 2H), 6.82 ~ 6.84(d, J = 8.7Hz, 2H), 7.13 ~ 7.17(m, 2H).
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