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Preparation method of surface amino-group functionalization SBA-15 mesoporous silica

A technology of mesoporous silica and amino functional group, which is applied in the preparation of silica and amino compounds, and the preparation of organic compounds, etc., can solve the problems of poor material morphology, uneven distribution, and embedding of functional groups, and achieve rich The effect of method type, uniform pore size distribution and high hydrothermal stability

Inactive Publication Date: 2015-08-19
CHENGDU INST OF BIOLOGY CHINESE ACAD OF S
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of the present invention is to solve the problems of functional group embedding, uneven distribution, poor order, pore blockage, too small pore size, and poor material morphology in the existing surface amine-functionalized SBA-15 synthesis method. A novel method suitable for one-pot synthesis of surface amine-functionalized SBA-15 under acidic conditions

Method used

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  • Preparation method of surface amino-group functionalization SBA-15 mesoporous silica
  • Preparation method of surface amino-group functionalization SBA-15 mesoporous silica
  • Preparation method of surface amino-group functionalization SBA-15 mesoporous silica

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Embodiment 1

[0033] (1) Synthesis of amino functional precursor protected by 2-naphthol (Np): Dissolve Np (1.44g, 10mmol) in 30mL anhydrous THF under nitrogen protection, add ICPTES (1.28mL, 5mmol), triethylamine (10mmol); Heating at 60°C for 24h, TLC detects that there is no raw material point, reclaims the solvent, and the resulting solid is recrystallized with n-hexane to obtain the precursor Np-Si; the reaction of the preparation of the 2-naphthol-protected amino functional precursor in this step The formula is as follows:

[0034]

[0035] (2) Synthesis of mesoporous silica material: at room temperature, P123 (1.85g, 0.32mmol) was dissolved in 3mol / L hydrochloric acid aqueous solution, wherein the molar ratio of acid, deionized water and structure directing agent was: 11.5 / 210 / 0.016, stirred for 2h to obtain a clear and transparent solution A. Weigh Np-Si (1.833g, 5mmol, accounting for 20% of the total silicon source) and dissolve it with 1mL THF to obtain solution B. At 40°C, add...

Embodiment 2

[0040] (1) Synthesis of functional precursors protected by phenol (Ph): under the protection of argon, dissolve Ph (0.94g, 10mmol) in 20mL of anhydrous toluene, add ICPTES (2.55mL, 10mmol), dilauric acid Dibutyltin (5 mmol). Heat at 60°C for 18 hours, TLC detects no raw material point, recover the solvent, and purify the obtained solid through a silica gel column to obtain the precursor Ph-Si; the reaction formula for the preparation of the phenol-protected amino functional precursor in this step is as follows:

[0041]

[0042] (2) Synthesis of mesoporous silica material: at room temperature, P123 (1.2g, 0.2mmol) was dissolved in 3mol / L nitric acid aqueous solution, wherein the molar ratio of acid, deionized water and structure directing agent was: 11.5 / 210 / 0.020, stir until a clear and transparent solution A is obtained. Weighed Ph-Si (0.213g, 0.67mmol) and dissolved it in 1mL THF to obtain solution B, and added solution B dropwise to rapidly stirring solution A at 35°C....

Embodiment 3

[0047] (1) Synthesis of 4-benzylphenol (Bp)-protected amino functional precursor: under nitrogen protection, Bp (1.84g, 10mmol) was dissolved in 30mL of anhydrous chloroform, and ICPTES (3.82mL, 15mmol) was added, 50 mmol piperidine. Heat at 60°C for 24 hours, TLC detects no raw material point, recover the solvent, and recrystallize the obtained solid with n-hexane to obtain the precursor Bp-Si; the reaction formula for the preparation of the 4-benzylphenol-protected amino functional precursor in this step is as follows:

[0048]

[0049] (2) Synthesis of mesoporous silica material: Dissolve P123 (0.93g, 0.16mmol) in 3mol / L sulfuric acid solution at room temperature, wherein the molar ratio of acid, deionized water and structure directing agent is: 11.5 / 210 / 0.020, stirred until clear and transparent to obtain solution A. Weighed Bp-Si (0.431g, 1.00mmol) and dissolved it in 1mL THF to obtain solution B, and added solution B dropwise to rapidly stirred solution A at 45°C. A...

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Abstract

The invention discloses a preparation method of surface amino-group functionalization SBA-15 mesoporous silica, and belongs to the technical field of organic functionalization ordered mesoporous materials synthetic method. The method comprises the following steps of taking aryl groups of different structures as protecting groups to react with silane coupling agents to prepare alkyl group trialkoxysilane functional precursor; under an acidic condition, taking tri-block non-ionic surface active agents as structure directing agents, and after pre hydrolyzing precursor, carrying out copolymerization with tetraethoxysilane or tetramethylsilane. The preparation method is characterized in that the aryl groups of different structures are taken as the protecting groups, so the functional precursor can be simply, conveniently and quickly prepared, and through the co-template role of the aryl groups and the structure directing agents, SBA-15 mesoporous silica, of which amino height is located at the inner surface of a duct, the microstructure is ordered and the bore diameters are different, is obtained.

Description

technical field [0001] The invention relates to a preparation method of amine functionalized SBA-15 mesoporous silica on the surface of pores, and belongs to the technical field of synthesis methods of organic functionalized ordered mesoporous materials. Background technique [0002] According to the definition of the International Union of Pure and Applied Chemistry (IUPAC), porous materials with a pore size between 2 and 50 nm are called mesoporous materials. Mesoporous materials have uniform and continuously adjustable pore size at the nanoscale, large specific surface area and pore volume, rich and diverse ordered mesoscopic structures and chemical compositions, controllable morphology, and easy functionalization of the surface And a series of advantages, so it is widely used in catalysis, adsorption and separation, chemical sensing, drug delivery, environmental protection and other fields. [0003] Since 1992, Mobil Corporation reported the synthesis of M41S (MCM-41, M...

Claims

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Application Information

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IPC IPC(8): B01J31/02B01J20/22B01J20/28B01J20/30A61K47/04A61K47/18C01B33/12C07C209/62C07C211/06
CPCY02P20/55
Inventor 王淳张国林李云萍罗贵桃
Owner CHENGDU INST OF BIOLOGY CHINESE ACAD OF S
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