Method for preparing hierarchical porous titanium silicalite TS-1
A technology of titanium silicalite, TS-1, applied in the field of preparation of multi-level porous titanium silicalite TS-1, to achieve the effect of reducing synthesis cost, simplifying the preparation process, and eliminating cumbersome processes
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[0023] Example 1
[0024] Take 1.5g of tetrapropylammonium bromide, 8ml of deionized water and 3.9ml (weight 30%) of silica sol and add 8.4g (weight 50%) of caramel solution in turn; take 0.16ml of tetrabutyl titanate to dissolve In 1.6ml isopropanol (volume ratio 1:10), mix well and slowly drop into the above solution. The molar ratio of tetrapropylammonium bromide, deionized water, silica sol and tetrabutyl titanate is composed Is 0.24:36.5:1:0.02, caramel and silica sol (with SiO 2 The resulting mixture is heated to 80°C and stirred for 2h; then the mixture is placed at 170°C for 28h to obtain a black solid dry gum. Grind the dry glue into a powder and place it in a container in the middle of the crystallization kettle, add 9ml of ethylenediamine and 12ml of water at the bottom; place the crystallization kettle at 170°C for 7d. After washing, filtering, and drying the obtained solid, it is calcined at 650° C. for 10 hours to obtain multi-stage TS-1. In the XRD pattern of the...
Example Embodiment
[0025] Example 2
[0026] Take 1.5g of tetrapropylammonium bromide, 8ml of deionized water and 3.9ml (weight 30%) of silica sol and add 2.8g (weight 50%) of caramel solution in turn; take 0.16ml of tetrabutyl titanate to dissolve In 1.6ml isopropanol (volume ratio 1:10), mix well and slowly drop into the above solution. The molar ratio of tetrapropylammonium bromide, deionized water, silica sol and tetrabutyl titanate is composed 0.24:30:1:0.02, caramel and silica sol (with SiO 2 The mass ratio is 1:1; the resulting mixture is heated to 80°C and stirred for 2h; then the mixture is placed at 170°C for 24h to obtain a black solid dry gum. Grind the dry glue into a powder and place it in a container in the middle of the crystallization kettle, add 9ml of ethylenediamine and 12ml of water at the bottom; place the crystallization kettle at 170°C for 7d. After washing, filtering, and drying the obtained solid, it is calcined at 650° C. for 10 hours to obtain multi-stage TS-1.
Example Embodiment
[0027] Example 3
[0028] Take 1.5g of tetrapropylammonium bromide, 8ml of deionized water and 3.9ml (weight 30%) of silica sol and add 5.6g (weight 50%) of caramel solution in turn; take 0.16ml of tetrabutyl titanate to dissolve In 1.6ml isopropanol (volume ratio 1:10), mix well and slowly drop into the above solution. The molar ratio of tetrapropylammonium bromide, deionized water, silica sol and tetrabutyl titanate is composed Is 0.24:33.3:1:0.02, caramel and silica sol (with SiO 2 The resulting mixture is heated to 80°C and stirred for 2h; then the mixture is placed at 170°C for 36h to obtain a black solid dry gum. Grind the dry glue into a powder and place it in a container in the middle of the crystallization kettle, add 9ml of ethylenediamine and 12ml of water at the bottom; place the crystallization kettle at 170°C for 7d. After washing, filtering, and drying the obtained solid, it is calcined at 650° C. for 10 hours to obtain multi-stage TS-1.
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