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Porous organic-inorganic composite material and method for preparing same

An inorganic composite material and organic technology, applied in the direction of silica, silicon oxide, etc., can solve the problems of large capillary size, harsh reaction conditions, and limited application range, and achieve the effects of convenient operation, easy-to-obtain raw materials, and easy purification

Active Publication Date: 2014-04-09
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These reports are grafting metal-organic complexes on the outer surface or inner surface of inorganic materials to form organic-inorganic composite materials for heterogeneous catalysts for olefin polymerization, but the grafting rate is low, the process is cumbersome, the reaction conditions are harsh, and the cost is high.
Feldmann et al. (Anke Feldmann, Ute Clauβnitzer, Matthias Otto. Optimization of capillary coating by hydroxylethyl methacrylate for capillary zone electrophoresis of proteins. Journal of Chromatography B, 2004, 803, 149-157) reported the grafting of functional organic macromolecules in quartz capillaries. Molecular technical solutions, however, the large size of the capillary limits its range of applications

Method used

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  • Porous organic-inorganic composite material and method for preparing same
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  • Porous organic-inorganic composite material and method for preparing same

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Embodiment 1

[0034] This embodiment provides a method for preparing a novel porous organic-inorganic composite material, which includes the following steps:

[0035] 1. Synthesis of functional organic compounds

[0036]Heat the dry Schrank tube to vacuum, replace nitrogen to remove oxygen, cool, take 20mL dichloromethane, 3.28mL (23.5mmol) triethylamine, 2.52mL butenol into the Schrank tube, and place in ice water Cool to 0°C, add bromoisobutyryl bromide dropwise, stir in an ice-water bath for 3 h, then stir at room temperature for 12 h; use a rotary evaporator to evaporate under reduced pressure, wash with 3N hydrochloric acid, and then wash with saturated NaHCO 3 aqueous solution, and finally with deionized water, followed by anhydrous Na 2 SO 4 Dried, passed nuclear magnetic detection, nuclear magnetic detection data: 1 H NMR (CDCl 3 , Me 4 Si): δ1.93(s, 6H), 2.42-2.48(m, 2H), 4.23(t, J=6Hz, 2H), 5.12(t, J=12Hz, 2H), 5.74-5.86(m, 2H ).) Determine the product structure as follows, ...

Embodiment 2

[0052] This embodiment provides a preparation method of a novel porous organic-inorganic composite material, which is grafted by direct reaction between the hydroxyl group on the surface of the silica vesicle and a functional group (such as a carboxyl group), and the reaction equation is as follows:

[0053]

[0054] The preparation method provided in this embodiment comprises the following steps:

[0055] 1. Add 1.2g of silica vesicle material (0.02mol) to a dry Schrank tube, vacuumize, heat to remove water, replace nitrogen to remove oxygen, and cool; add 30ml THF, 0.66g, to the Schrank tube α-Bromoisobutyric acid (0.004mol), heated to 87°C in an oil bath, and refluxed for 15h;

[0056] 2. Stop heating, wait for the Schrank tube to cool down, transfer the mixture in the tube to a centrifuge tube and add acetone for centrifugation (3500r / min, 3min), remove the supernatant, then wash with acetone, centrifuge, repeat 5 times;

[0057] 3. Remove volatile substances under red...

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Abstract

The invention relates to a porous organic-inorganic composite material and a method for preparing the porous organic-inorganic composite material. The method comprises the following steps: subjecting a compound of formula (1) and a compound of formula (2) to reaction in the methylene dichloride solvent in the alkaline environment provided by the triethylamine to generate a compound of formula (3), subjecting the compound of formula (3) to reaction with a compound of formula (4) under the catalysis of the Pt which serves as a catalyst to generate a functional organic compound of formula (5), subjecting the functional organic compound of formula (5) to reaction with the porous-silicon based vesicle material to generate an organic-inorganic composite material, filtering the organic-inorganic composite material, washing by a washing solvent, and drying in vacuum to obtain the porous organic-inorganic composite material. The raw materials adopted by the method for preparing the porous organic-inorganic composite material are easy to obtain, and the functional compound is easy to synthesize, has high reaction yield and is easy to purify.

Description

technical field [0001] The invention relates to a porous organic-inorganic composite material and a preparation method thereof, belonging to the technical field of material preparation. Background technique [0002] Porous materials such as zeolite, molecular sieve, activated carbon, kaolin, etc. are widely used in the fields of adsorption separation, catalysis, drug release, sensor, etc., and because of their unique physical and chemical properties, such as low density, large specific surface area and large internal Space etc. are getting more and more attention. [0003] In recent years, in the continuous exploration of the preparation of ordered mesoporous materials, researchers have discovered materials with vesicle structure. Vesicular materials not only have large pore size and large pore volume, but also have broad application prospects in adsorption separation, catalyst carrier, drug sustained release, pigment microreactor, etc. [0004] Modification of these mesop...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/12
Inventor 任申勇闫慧申宝剑郭巧霞
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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