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

Active Publication Date: 2017-02-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there are many materials synthesized with silicon-based mesoporous materials as substrates and mercapto groups as modification groups, but there are few studies on the modification of organic mesoporous silicone materials with polysulfides.

Method used

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  • A modified ordered mesoporous organosilicon material and its preparation method and application
  • A modified ordered mesoporous organosilicon material and its preparation method and application
  • A modified ordered mesoporous organosilicon material and its preparation method and application

Examples

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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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Abstract

The present invention discloses a modification method of an ordered mesoporous organosilicon material (PMO), the PMO prepared by the method, and application of the PMO as an adsorbent. The method comprises the following steps: first dispersing the ordered mesoporous organosilicon material into an organic solvent to prepare a suspension, and then contact bis (triethoxysilyl)-alkyl polysulfide with the suspension under hydrolysis condensation reaction conditions. The bis (triethoxysilyl)-alkyl polysulfide has a general formula (C2H5O)3Si-R-Sx-R'-Si (OC2H5)3, wherein R and R' respectively represent C1-C10 alkylene, and x equals to 2; preferably, R and R respectively represent C1-C5 alkylene, and x satisfies the relation of 4>x>2; more preferably R and R respectively represent propylidene, and x equals to 4 or 2. The modified mesoporous organosilicon material prepared by the method of the invention has excellent adsorption selectivity performance on heavy metal mercury ions in water.

Description

technical field [0001] The invention relates to a preparation method of a modified ordered mesoporous organic silicon material, a modified ordered mesoporous organic silicon material prepared by the method, and an application of the modified ordered mesoporous organic silicon material as an adsorption material. Background technique [0002] In 1992, Mobil Corporation synthesized the M41S mesoporous molecular sieve series materials with ordered pore structure for the first time. Since then, mesoporous materials have been favored by scientists for their ordered pore structure and large specific surface area. focus on. With the development of mesoporous materials, a very unique mesoporous material-ordered mesoporous silicone material was born. In just a few years, the diversity of pore wall structures has once again set off research on mesoporous materials. upsurge. From the perspective of hybrid materials, ordered mesoporous organosilicon materials are very useful materials,...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C08G77/28C08G77/06C08L83/08B01J20/26
Inventor关敏毕海鹏邵明波王足远卜少华黄铃杨力
OwnerCHINA PETROLEUM & CHEM CORP