A camphorsulfonamide-doped ethane bridge spherical mesoporous silica gel

A mesoporous silica gel, sulfonamide technology, applied in other chemical processes, chemical instruments and methods, etc., can solve the problems of harsh conditions, difficult to control the uniformity of organic group distribution, and complex processes

Inactive Publication Date: 2011-12-14
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The conditions of this reaction are harsh, the process is complicated, and it is difficult to control the uniform distribution of organic groups on the surface of silica gel.

Method used

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  • A camphorsulfonamide-doped ethane bridge spherical mesoporous silica gel
  • A camphorsulfonamide-doped ethane bridge spherical mesoporous silica gel
  • A camphorsulfonamide-doped ethane bridge spherical mesoporous silica gel

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Synthesis of Camphorsulfonamide-doped Spherical Mesoporous Silica Gel with Ethane Bridges

[0030] Take by weighing 0.94g octadecyltrimethylammonium chloride in a 100ml round bottom flask, add deionized water (21.0ml), ethanol (18.0ml) and sodium hydroxide solution (1M, 13.5ml) successively, stir vigorously to make Mix well to obtain a clear and transparent solution. The ethanol solution of 1,2-bis(triethoxysilyl)ethane (1.59g) and camphorsulfonamide derivative silicon ester I (0.39g) mixed uniformly was added dropwise to the above-mentioned transparent solution, at room temperature Stirring was continued for 1 hour, and then the reaction solution was transferred to a reaction kettle and stood at 90° C. for 18 hours, filtered, thoroughly washed with deionized water, and dried to obtain a solid material. Mix 1 g of solid material with 200 ml of acidic ethanol and extract at 60°C for 6 hours to remove the template agent, filter, wash and dry to obtain camphorsulfonamide-...

Embodiment 2

[0032] Application of Camphorsulfonamide-doped Spherical Mesoporous Silica Gel as Chromatographic Stationary Phase

[0033] Get the camphorsulfonamide-doped ethane bridge bonded spherical mesoporous silica gel prepared in Example 1, use the homogenization method to fill in a stainless steel column tube (150mm × 4.6mm, I.D.), the column packing pressure is 40MPa, and use this chromatographic The column was tested for chromatographic separation. A Shimadzu LC-20AT high performance liquid chromatograph and an SPD-20A ultraviolet detector were selected, and the probe molecules were selected from benzene, anthracene and nitrobenzene, all of which were prepared into a solution of about 200 μg / ml with n-hexane as a solvent, and the injection volume was 20 μL. The mobile phase is n-hexane, the flow rate is 1ml / min, and the detection wavelength is 254nm. The three compounds can achieve baseline separation. Chromatogram see Figure 8 .

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Abstract

The invention relates to the technical fields of ordered mesoporous materials and analytical chemistry, and discloses camphor sulfonamide doped ethane bridge bond spherical mesoporous silica gel and a preparation method thereof. The silica gel is prepared by taking a cationic surfactant as a structure directing agent and taking a camphor sulfonamide derivative and 1,2-di(triethoxysilane) as a mixed silicon source in the presence of alkali and an organic cosolvent. Camphor sulfonamide organic radicals are bonded in pore passages of the material; and ethylene groups are bonded in a framework. The silica gel has a simple preparation process; the organic radicals are uniformly distributed in the pore passages and pore walls in a covalent bond mode; the material has high specific surface area of 500-1,000m<2>/g and uniform and adjustable ordered aperture of 2-10nm and is microsphere with the aperture of 5-7mum. The organic-inorganic mesoporous silica gel can be used as a liquid-phase chromatographic stationary phase.

Description

technical field [0001] The invention belongs to the technical field of preparation and analytical chemistry of ordered mesoporous materials, and in particular relates to a spherical mesoporous silica gel doped with ethane bridge bonds by camphorsulfonamide and a preparation method thereof. The silica gel can be used as a chromatographic stationary phase filler. Background technique [0002] Bonded stationary phases are commonly used in traditional liquid chromatography, and the preparation process usually involves the reaction of silanol groups on the surface of silica gel with coupling agents, and then introducing organic functional groups to the surface of silica gel. The conditions of this reaction are harsh, the process is complicated, and it is difficult to control the uniformity of the distribution of organic groups on the surface of silica gel. [0003] Organic-inorganic hybrid mesoporous silica with bridging organic functional group disiloxane——(R′O) 3 Si-R-Si(OR') ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/28C08J9/26B01J20/283B01J20/30
Inventor 狄斌鲁涓
Owner CHINA PHARM UNIV
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