Method for preparing hydrophobic silicon dioxide
A silicon dioxide and hydrophobic technology, applied in the direction of inorganic compound addition, dyeing organosilicon compound treatment, dyeing physical treatment, etc., can solve the problem of unsatisfactory high hydrophobicity, and achieve the goal of preventing self-condensation and self-condensation reaction Effect
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[0071] In the preparation of the hydrophobized silica of the present invention, it is sometimes necessary to store the hydrophobic silica fine particles for a long time until they are actually used, and during this storage, hydrophobic silica particles may be generated. Agglomeration of powder. Hydrophobic silica with good dispersibility can be obtained by adding a fluorine-based surfactant when hydrophobizing reaction with hydrophilic silica. As the fluorine-based surfactant, there are fluorine-based compounds represented by the general formulas (3) to (5). In general formula (3), R 7 It is a perfluoroalkyl group with 5 to 8 carbon atoms, A is COOM, SO 3 M base, M is Na, K, Li. In general formula (4), R 8 It is a perfluoroalkyl group with 5 to 18 carbon atoms, and Y is H (hydrogen atom), -OPO(OH) 2 (phosphate residue), and p is an integer of 1-15. In general formula (5), R 9 is a perfluoroalkyl group having 5 to 18 carbon atoms, Z is a chlorine atom, a bromine atom, an...
Embodiment 1
[0106] Hydrophobic silica 1 of Example 1 was prepared as follows.
[0107] Add 70 parts by weight of higher alcohol emulsion (B-1), 70 parts by weight of water, and 10 parts by weight of alkylsilane compound (A-1) and stir for 40 minutes to prepare a higher alcohol emulsion with hydrolyzate of alkylsilane compound adsorbed on the surface. Add 100 parts by weight of hydrophilic silicon dioxide (C-1) to a reactor with a stirrer, a thermometer and a condenser, and slowly add a higher alcohol emulsion with a hydrolyzate of an alkylsilane compound adsorbed on the surface under stirring, and evenly coated on hydrophilic silica. The reactor was heated to 110° C. to 130° C. while stirring, and the temperature was maintained for 60 minutes, after which water was removed to obtain hydrophobic silica 1 .
Embodiment 2
[0109] Hydrophobic silica 2 of Example 2 was prepared as follows.
[0110] In Example 1, 100 parts by weight of the hydrophilic silica (C-1) was sprayed with a higher alcohol emulsion with alkylsilane compound hydrolyzate adsorbed on the surface under stirring, and evenly coated on the hydrophilic silica superior. The reactor was heated to 110°C to 130°C, and water was evaporated while maintaining the temperature to obtain hydrophobic silica 2.
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