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Cholesterol derivatives and o/w/o heterogeneous gel emulsions prepared therefrom and methods for preparing porous silica blocks using the emulsions

A technology of cholesterol derivatives and gel emulsions, applied in the direction of silica, silicon oxide, organic chemistry, etc., to achieve the effects of good stability, good adsorption performance, and regular pore structure

Inactive Publication Date: 2016-07-27
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 derivatives and o/w/o heterogeneous gel emulsions prepared therefrom and methods for preparing porous silica blocks using the emulsions
  • Cholesterol derivatives and o/w/o heterogeneous gel emulsions prepared therefrom and methods for preparing porous silica blocks using the emulsions
  • Cholesterol derivatives and o/w/o heterogeneous gel emulsions prepared therefrom and methods for preparing porous silica blocks using the emulsions

Examples

Experimental program
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Effect test

Embodiment 1

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

[0049]

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

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

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 vinyl triethoxy silane, 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 Phase gel emulsion (see figure 1 with figure 2 ), it can be seen from the figure that the size of the droplets in the obtained multiphase gel emulsion is uniform, showing the characteristics of solid.

Embodiment 3

[0060] Preparation of O / W / O multiphase gel emulsion

[0061] In Example 2, the vinyl triethoxy silane used was replaced with an equal volume of 3-chloropropyl triethoxy silane, and the other steps were the same as in Example 2, to obtain an O / W / O heterogeneous gel emulsion (see image 3 with 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 block method. Background technique [0002] Multiphase emulsion is a multi-layer emulsion formed by dispersing an emulsion (usually called primary emulsion, or colostrum for short) in another continuous phase. It is generally a highly dispersed multiphase system with different particle sizes. There are many types, the most common are W / O / W and O / W / O. In terms of structure, the multiphase emulsion has a unique "two-membrane three-phase" multi-compartment structure, such as O / W / O type multiphase emulsion, which contains one or more oil droplets in the water droplets. The water droplets are dispersed in the oil phase to form an emulsion. It is precisely because of the special structure of multiphase emulsion that some substances with different ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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