A kind of multiple responsive pickering emulsion and preparation method thereof
A multi-response, emulsion technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxy compounds, etc., can solve the problems of thermodynamic instability, high concentration of surfactants, and difficulty in breaking emulsions.
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Embodiment 1
[0058] Example 1: Preparation of surfactant N-8P-N +
[0059] Surfactant N-8P-N + The synthetic route is as follows:
[0060]
[0061] (1) acyl chlorination reaction: 8-bromooctanoic acid solid (30g, 0.135mol) is added to the there-necked flask that the device for tail gas absorption, the reflux of condenser tube are housed, and three drops of N,N-dimethylformamide (DMF) are added. ) as a catalyst, thionyl chloride (21 g, 0.178 mol) was slowly added dropwise. The reaction temperature was 60 °C, the reaction was performed for 1 h, and the excess thionyl chloride was removed by a rotary evaporator to obtain the intermediate I.
[0062] (2) Amidation reaction: Place dimethylamine hydrochloride (14g, 0.172mol) and triethylamine (50g, 0.494mol) in a low temperature reactor at -10°C, dropwise add Intermediate I (32.61g, 0.135mol) ) in dichloromethane solution, react for 2h after the end, and then extract the reaction solution with water for more than three times to remove exc...
Embodiment 2
[0067] Example 2: Nano-SiO 2 Surface activity test of particles
[0068] In a 25mL glass bottle, weigh 0.007g of commercial nano-SiO 2 Particles (primary particle size is about 20nm, specific surface area S BET About 200±20m 2 / g, see SEM and TEM images figure 2 ), add 7 mL of ultrapure water, and then use an ultrasonic disperser to disperse the particles uniformly. The mass fraction of particles was 0.1% (relative to the aqueous phase). Add 7mL of n-decane to the glass bottle, and then use a high shear homogenizer to rotate and emulsify at 11000r / s for 2min, such as image 3 , a stable emulsion could not be obtained, indicating that the commercial nano-SiO used 2 The particles are not surface active.
Embodiment 3
[0069] Example 3: Preparation of Pickering Emulsion
[0070] Weigh 0.007g of nano-SiO 2 The particles were ultrasonically dispersed in 7mL of N-8P-N with different concentrations +7 mL of n-decane was added to the solution, and after homogeneous emulsification with a high shear homogenizer for 2 min, a stable O / W Pickering emulsion was obtained. like Figure 4 As shown, after the emulsion was placed for one month, no emulsification or demulsification occurred, indicating that the obtained Pickering emulsion had very good stability.
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