All-silicon mesoporous material, preparation method thereof and application thereof in rearrangement reaction

[0019] The second aspect of the present invention provides a method for preparing an all-silicon mesoporous material, the method comprising:

[0020] (1) Mix acid, surfactant and organosilicon source to SiO 2 Calculated organic silicon source, with H + The molar ratio of the amount of the acid, the surfactant and the water is 100:0.1-50:0.01-20:200-50000; a mixture with the hydrolysis rate of the organosilicon source being 20% ​​by weight or less is obtained;

[0021] (2) Under airtight conditions, subject the mixture obtained in step (1) to crystallization treatment; wherein, the conditions of the crystallization treatment include: a temperature of 60-190°C and a time of 4-100h;

[0022] (3) Solid-liquid separation is performed on the product after the crystallization treatment, and the solid phase obtained by the solid-liquid separation is calcined.

[0023] According to the present invention, the preparation method of the all-silicon mesoporous material of the present invention can obt

[0048] Example 1

[0049] This embodiment is used to illustrate the all-silicon mesoporous material of the present invention and its preparation method.

[0050] First add 50g of ethyl orthosilicate and cocamidopropyl dimethyl tertiary amine (purchased from Huainan Dejun Fine Chemical Co., Ltd.) into the aqueous solution of hydrochloric acid and mix (mix for about 2 minutes at 20°C), in which ethyl orthosilicate The molar ratio of ester, hydrochloric acid, cocamidopropyl dimethyl tertiary amine and water is 1:1:1:1000, and the organic silicate is SiO 2 Calculated, acid source in H + Calculate, and immediately transfer the resulting mixture (hydrolysis rate of organosilicon source below 5%) into a sealed reactor for hydrothermal crystallization at 120°C for 10 hours, filter, wash, and dry the resulting crystalline product at 110°C for 120 minutes, then It was fired at 550°C for 3 hours to obtain mesoporous silicon material A1.

[0051] After testing, its XRD crystal phase has diffractio

[0052] Example 2

[0053] This embodiment is used to illustrate the all-silicon mesoporous material of the present invention and its preparation method.

[0054] First add 50g of ethyl orthosilicate and lauramidopropyl dimethyl tertiary amine (purchased from Huainan Dejun Fine Chemical Co., Ltd.) into the aqueous solution of acetic acid and mix (mix for about 1 min at 20°C), in which ethyl orthosilicate The molar ratio of acetic acid, lauramide propyl dimethyl tertiary amine and water is 1:1.5:1.5:800, and the organic silicate is SiO 2 Calculated, acid source in H + Calculate, and immediately transfer the obtained mixture (hydrolysis rate of organosilicon source below 3%) into a sealed reaction kettle for hydrothermal crystallization at 140°C for 12h, filter, wash, and dry at 110°C for 100min, then It is fired at 560°C for 4h to obtain mesoporous silicon material A2.

[0055] After testing, its XRD crystal phase has diffraction peaks at small angles, namely 2θ near 0.8°, 1.5° and 1.7°,