Preparation method of organosilicon compound grafted silica
A technology of organosilicon compounds and silicon dioxide, applied in the directions of organosilicon compounds, chemical instruments and methods, chemical/physical processes, etc., can solve problems such as expensive anti-corrosion equipment
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Embodiment 1
[0140] Embodiment 1: Preparation of silica grafted with non-functionalized cyclotetrasiloxane according to the present invention
[0141] The process described below was carried out in a 3 L reactor equipped with a twin shaft stirrer and baffles.
[0142] First, add 800g of deionized water to a 3L reactor; 120g of Aerosil © A200 fumed silica is dispersed in water.
[0143] Then, 400.9 g of deionized water was added, followed by 0.9197 g of NaCl salt. Stirring speed was reduced to 200 rpm overnight.
[0144] 6 ml of soda solution at about 1 mol / l was added to achieve a near neutral pH. Although the dispersed phase was not completely liquid as it formed a gel, the pH of the gel was measured to be about 7.2.
[0145] Then, 399.2 g of isopropanol (IPA) was added, followed by 270.4 g of octamethylcyclotetrasiloxane (D 4 ). The intermediate was refluxed for 24 hours at 600 rpm stirring speed and 80°C. A kinetic study was carried out showing that grafting indeed occurs coval...
Embodiment 2
[0147] Example 2: Preparation of silica grafted with non-functionalized cyclotetrasiloxane according to the present invention (Example 2)
[0148] Implementation method is similar to that described in Example 1, adopting 170g Aerosil © A200 fumed silica, 1700g deionized water, 1.3029g NaCl and 202g IPA. Soda was then added to achieve a pH of 7.3.
[0149] Then, 362.2g IPA was added, followed by 383.01g D 4 . After 24 h at 80 °C, filter the silica with a filter plate (pore diameter: 20 µm) at 2 bar pressure. The silica remaining in the reactor is then recovered with a biphasic water / heptane mixture; only the heptane phase is recovered and filtered to recover all the silica.
[0150] Then, the filtered silica was placed in an oven and dried under vacuum at 90°C for 48 hours. The dried silica is placed in a tank and the silica clusters are mechanically broken.
Embodiment 3
[0151] Example 3: Preparation of silica grafted with non-functionalized cyclotetrasiloxane according to the present invention (Example 3)
[0152] The same operation process as in Example 1 was adopted. The only difference is that the heating time is halved, i.e. reflux at 80°C for 12 hours instead of 24 hours.
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