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Cholesterol derivative, O/W/O multi-phase gel emulsion prepared from cholesterol derivative, and method for preparing porous silicon dioxide bulk material from emulsion

A technology of cholesterol derivatives and gel emulsions, applied in the fields of silica, silicon oxide, organic chemistry, etc., to achieve the effect of simple method, simple preparation method and low density

Inactive Publication Date: 2015-09-09
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, at present, the preparation of porous blocks using emulsions as templates is mainly concentrated in the research of polymer blocks. Using this method to obtain SiO 2 The study of porous bulk materials has not been reported, and the simple, convenient and low-cost controllable preparation of structurally rich SiO 2 Porous bulk materials are currently SiO 2 The bottleneck of porous bulk materials towards application

Method used

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  • Cholesterol derivative, O/W/O multi-phase gel emulsion prepared from cholesterol derivative, and method for preparing porous silicon dioxide bulk material from emulsion
  • Cholesterol derivative, O/W/O multi-phase gel emulsion prepared from cholesterol derivative, and method for preparing porous silicon dioxide bulk material from emulsion
  • Cholesterol derivative, O/W/O multi-phase gel emulsion prepared from cholesterol derivative, and method for preparing porous silicon dioxide bulk material from emulsion

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Experimental program
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Embodiment 1

[0048] To synthesize cholesterol derivatives, the specific synthetic route and synthetic method are as follows:

[0049]

[0050] 1. Preparation of the compound of formula 2-1

[0051] Under nitrogen protection, add 20mL tetrahydrofuran and 14.29mL (77.5mmol) 1,8-dibromooctane to the three-necked flask, then add 3.48g (62mmol) finely ground KOH; dissolve 6g (15.5mmol) cholesterol in 30mL THF, and then add it dropwise into a three-necked flask, and react at 80°C for 48 hours. After the reaction, remove the KOH solid by filtration, remove THF by rotary evaporation, extract with dichloromethane, remove dichloromethane by rotary evaporation, and use methanol Recrystallization (3 times) to obtain white crystals, using a mixed solution of petroleum ether and methylene chloride with a volume ratio of 1:1 as a developing solvent, separated by silica gel column chromatography to obtain a compound of formula 2-1, and its structural characterization result is : 1 H-NMR (400MHz, CDCl...

Embodiment 2

[0057] Preparation of O / W / O Multiphase Gel Emulsion

[0058] Dissolve 0.15 g of the cholesterol derivative prepared in Example 1 in 1 mL of vinyltriethoxysilane, add 4 mL of distilled water, and stir mechanically at room temperature for 2 minutes at a speed of 11400 rpm to obtain O / W / O poly Phase gel emulsion (see figure 1 and figure 2 ), it can be seen from the figure that the droplet size in the resulting heterogeneous gel emulsion is uniform, showing the characteristics of a solid.

Embodiment 3

[0060] Preparation of O / W / O Multiphase Gel Emulsion

[0061] In Example 2, the vinyl triethoxysilane used was replaced with an equal volume of 3-chloropropyl triethoxysilane, and the other steps were the same as in Example 2 to obtain an O / W / O heterogeneous gel emulsion (See image 3 and Figure 4 ).

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Abstract

The invention discloses a cholesterol derivative, an O / W / O multi-phase gel emulsion prepared from the cholesterol derivative, and a method for preparing a porous silicon dioxide bulk material from the emulsion. The structural formula of the cholesterol derivative is as shown in the description, wherein n is an integer of 6 to 12, and R represents a C1-C4 alkyl group. The O / W / O multi-phase gel emulsion is prepared according to a one-step method by taking the cholesterol derivative as a sing surfactant and taking a silanization reagent as an oil-phase material, and is high in stability, stable to acid and alkali, uniform in droplet distribution, and high in water-phase content which is 80 to 97 percent of the total volume. The porous silicon dioxide bulk material is prepared by taking the O / W / O multi-phase gel emulsion as a template at an ammonia gas atmosphere. The method is simple and low in cost; the prepared silicon dioxide bulk material is low in density, and has rich hierarchical porous structures which are regular and high in permeability; moreover, the porous silicon dioxide bulk material is large in surface area, high in heat stability, adjustable in hydrophilicity and hydrophobicity, and excellent in water or oil adsorption property.

Description

technical field [0001] The invention relates to a small molecule surfactant-cholesterol derivative, an O / W / O multiphase gel emulsion prepared by using the surfactant, and a porous O / W / O multiphase gel emulsion prepared as a template Silica bulk method. Background technique [0002] Multi-phase emulsion is a multi-layer emulsion formed by dispersing an emulsion (usually called primary emulsion, colostrum for short) in another continuous phase. It is generally a multi-phase system with high dispersion and different particle sizes. There are many types, the most common of which are W / O / W and O / W / O. In terms of structure, the multi-phase emulsion has a unique "two-film three-phase" multi-compartment structure, such as the O / W / O type multi-phase emulsion, which contains one or more oil droplets in the water droplet. The water droplets are dispersed in the oil phase to form an emulsion. Because of the special structure of the multiphase emulsion, some substances with different ...

Claims

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Application Information

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IPC IPC(8): C07J9/00C01B33/12
CPCC01B33/12C07J9/00
Inventor 彭军霞张媛媛杜冠群张红霞
Owner SHAANXI NORMAL UNIV
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