A modified ordered mesoporous organosilicon material and its preparation method and application
A mesoporous organosilicon, organosilicon technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problem of little research on modification, and achieve the effect of improving adsorption performance
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preparation example Construction
[0018] The invention provides a method for preparing a modified ordered mesoporous organic silicon material. The method comprises: firstly dispersing the ordered mesoporous organic silicon material in an organic solvent to prepare a suspension, and then under the conditions of hydrolysis and condensation reaction, the A bis(triethoxysilyl)-alkyl polysulfide is contacted with the suspension; the general formula of the bis(triethoxysilyl)-alkyl polysulfide is (C 2 h 5 O) 3 Si-R-S x -R'-Si(OC 2 h 5 ) 3 , wherein R and R' are each C1-C10 alkylene, x≥2; preferably, R and R' are each C1-C5 alkylene, 4≥x≥2; more preferably, R and Each R' is a propylene group, and x=4 or 2. Specifically, the bis(triethoxysilyl)-alkyl polysulfide can be bis-[3-(triethoxysilyl)propyl]disulfide, bis-[3-(triethoxy At least one of trisulfide and bis-[3-(triethoxysilyl)propyl]tetrasulfide, most preferably bis-[3-(triethoxysilyl)propyl] base]tetrasulfide and / or bis-[3-(triethoxysilyl)propyl]disulfide...
preparation example 1
[0039] The PMO material used in the following examples is prepared according to the following method:
[0040] At 40°C, 1 g of P123 (purchased from sigma-Aldrich) was dissolved in 2.98 g of 1.0 mol L -1 In the KCl aqueous solution, add 40g concentration to it again and be 0.167mol L -1 hydrochloric acid solution, and then 1.40 g of BTME (purchased from sigma-Aldrich) was added to the mixed solution and stirred. Stirring was stopped after 10 minutes, and the reaction system was left standing at 40° C. for 1 day. Subsequently, the mixture was transferred to an autoclave, and reacted at 100° C. for 24 hours. After the reaction, the solid product was collected by filtration and dried at room temperature. Finally, the solid product was subjected to Soxhlet extraction with ethanol to obtain the PMO material.
Embodiment 1
[0042] This example is used to illustrate the modified PMO material of the present invention and its preparation method.
[0043] Disperse 1.0 g of the ordered mesoporous organosilicon PMO material prepared in Preparation Example 1 uniformly in 20 ml of absolute ethanol at room temperature, stir to disperse evenly to obtain a suspension, and then add bis-[ 3-(triethoxysilyl) propyl] tetrasulfide (purchased from Bailingwei Technology Co., Ltd., the molecular formula is C 18 h 42 o 6 S 4 Si 2 ), wherein, according to the mass ratio, ordered mesoporous organosilicon PMO material: bis-[3-(triethoxysilyl)propyl]tetrasulfide=1:4.3, and then added to the reaction system under stirring Concentrated ammonia water with a concentration of 36% was used to adjust the pH so that the pH was 8. After the addition was complete, the reaction system was stirred and reacted at 40°C for 24 hours under the protection of nitrogen. After washing with water and acetone, the washed solid product w...
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