Method for preparing radial titanium dioxide nanorod coated silica gel core-shell structure microspheres through in-situ growth
An in-situ growth, radial technology, applied in the direction of silicon dioxide, titanium dioxide, silicon oxide, etc.
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Embodiment 1
[0018] 1 Activated silica gel: 0.8 g of porous silica gel (particle diameter is 4 μm) is soaked with concentrated hydrochloric acid for activation treatment 36 h, and then washed with deionized water to neutral, 120 ° C is dried 11 h to obtain an activated silica glue;
[0019] 2 Preparation of a crystal layer: 3 ml of titanate titanate is added dropwise to 50 mL of anhydrous ethanol, resulting in a seed solution, incorporating the activated porous silicone, 100 W Ultrasound 20 min , 500 rpm, allowing the seed solution to be uniformly attached to the surface of the silica gel, centrifuge, 80 ° C for 10 h, repeated attachment process 3 times; finally put silicone into the muffle 400 ° C 4 h, annealed After the surface of the silicone surface attached to a layer of TiO 2 Seed layer;
[0020] 3 Hydrotic / solvent thermal in situ: 3 ml of tetrabutyl titanate is added to 60 ml of water toluene to give tetrabutyl tetrabutyl titanate, and the step 2 has a crystal silica gel that has a cr...
Embodiment 2
[0022] 1 Activated silica gel: 1.0 g of porous silica gel (3 μm having a particle diameter) was soaked with concentrated hydrochloric acid for activation treatment 42 h, and then washed with deionized water to neutral, 110 ° C was dried 12 h, and the silica glue was obtained.
[0023] 2 Preparation of a crystal layer: 3 mL of titanate titanate was added dropwise to 50 mL of anhydrous ethanol, resulting in a seed solution, adding the activated porous silicone, 100 W Ultrasound 25 min. , 500 rpm is 1.5H, allowing the seed solution to be uniformly attached to the surface of the silica gel, centrifuge, 80 ° C for 10 h, repeated attachment process 3 times; finally put silicone into the muffle furnace 450 ° C 5 h, annealed After the surface of the silicone surface attached to a layer of TiO 2 Seed layer;
[0024] 3 Hydrotic / solvent thermal in situ growth: 4 ml of titanate tetrabutyate was added to 80 ml of water toluene to give tolukate solution, and the step 2 was added to the silica...
Embodiment 3
[0026] 1 Activated silica gel: The activation treatment of 1.3 g of porous silica gel (5 μm) was soaked with concentrated hydrochloric acid, and then washed with deionized water to neutral, and then dried 10 h after 120 ° C to obtain an activated silica glue;
[0027] 2 Preparation of a crystal layer: 4 ml of titanate titanate is added dropwise to 60 mL of anhydrous ethanol, resulting in a seed solution, and adds the activated porous silicone, 100 W Ultrasound 30 min. 500 rpm, allowing the seed solution to be uniformly attached to the surface of the silica gel, centrifuged, 80 ° C for 10 h, and then add silicone into the muffle furnace 500 ° C until 6 h, annealed After the surface of the silicone surface attached to a layer of TiO 2 Seed layer;
[0028] 3 Hydrotic / solvent thermal in situ growth: 5 ml of titanate tetrabutyate was added to 100 ml of water-free toluene to give tetrabutyl tetrabutyl titanate, and the step 2 was added to the silica gel therebetween. In the solution, ...
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