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A direct preparation of sio 2 Airgel Monolithic Column Method

An airgel and monolithic column technology, which is applied in the field of nanomaterial doping, can solve the problems of high production cost and achieve the effects of small reaction temperature change, low working pressure and large specific surface area

Active Publication Date: 2021-11-12
HOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of monolithic column has been developed rapidly in recent years due to the advantages of wide material selection, wide application range of pH value and simpler preparation compared with silica gel monolithic column, but its production cost is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Direct preparation of SiO 2 C1 airgel monolith, comprising the steps of:

[0044] 1. Weigh 0.7 g of double dodecyl dimethyl bromide (DDAB), placed in the reactor (25 ml of beaker);

[0045] 2. Take 3.5 ml of tetraethyl orthosilicate (TEOS) in the reactor;

[0046] 3. Take 3.5 mL of n-dodexecane into the reactor;

[0047] 4, take 0.7mL benzylamine pour into the reactor;

[0048] 5, ultrasonic dissolution as an oil phase;

[0049] 6, Al 2 (SO 4 ) 3 * 18h 2 O Soluble in water, concentration of 0.000112049 mol / ml, as aqueous phase;

[0050] 7, the 7ml aqueous phase is mixed with a 7 ml of oil phase, and the pore diameter is 5 μm, the inner diameter is 4.6mm, the column length is 150mm, and the empty liquid chromatography column is a double continuous microemulsion (very critical, to ensure injection The entire liquid is mixed milky white, no stratification, no bubbles, no liquid detention);

[0051] 8, stand for 24h under normal temperature conditions;

[0052] 9,70 ° C is dry...

Embodiment 2

[0057] Directly prepare SIO 2 The method of airgel integer column C2, including the steps of:

[0058] 1. Weigh 0.7 g of double dodecyl dimethyl bromide (DDAB), placed in the reactor (25 ml of beaker);

[0059] 2, take 3.5ml of the methyl sshalate pour into the reactor;

[0060] 3. Take 3.5 mL of n-dodexecane into the reactor;

[0061] 4, take 0.7mL benzylamine pour into the reactor;

[0062] 5, ultrasonic dissolution as an oil phase;

[0063] 6, Zn (no 3 ) 2 * 6h * 2 O Soluble in water, concentration of 0.000336146 mol / ml, as aqueous phase;

[0064] 7. The aqueous phase and the oil phase flow rate will be 1: 1, and the pore diameter is 5 μm and the inner diameter is 4.6 mm, the column length is 150 mm, and the empty liquid chromatography column is formed;

[0065] 8, stand for 24h under normal temperature conditions;

[0066] 9, 60 ° C under oxygen conditions for 24 h;

[0067] 10,600 ° C Heating under the conditions of oxygen;

[0068] 11,50ml thin hydrochloric acid soaked for...

Embodiment 3

[0071] Directly prepare SIO 2 Method for airgel integer column C3, including the following steps:

[0072] 1. Weigh 0.7 g of double dodecyl dimethyl bromide (DDAB), placed in the reactor (25 ml of beaker);

[0073] 2. Take 3.5 ml of tetraethyl orthosilicate (TEOS) in the reactor;

[0074] 3. Take 3.5 mL of n-dodexecane into the reactor;

[0075] 4, take 0.7mL benzylamine pour into the reactor;

[0076] 5, ultrasonic dissolution as an oil phase;

[0077] 6, Al 2 (SO 4 ) 3 * 18h 2 O Soluble in water, concentration of 0.000112049 mol / ml, Mg (NO 3 ) 2 * 6h * 2 O Soluble in water, concentration of 0.000289728 mol / ml, as aqueous phase;

[0078] 7, rapidly mixing 7 ml of aqueous phase with 7 ml of oil, and injects 5 μm in the pore diameter, a inner diameter of 4.6 mm, a column length of 150 mm, an empty liquid chromatography column, and is a double continuous microemulsion;

[0079] 8, standing for 24 hours under normal temperature conditions ;;

[0080] 9,80 ° C is dry under aerobic...

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PUM

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Abstract

The invention discloses a method for directly preparing SiO 2 The method of the airgel monolithic column belongs to the technical field of material separation and analysis, 1) adding silicate, basic organic matter, and surfactant to the organic solvent of the oil phase, and ultrasonically dissolving it as the oil phase; 2) dissolving the metal salt in Water, as the water phase; 3) Mix the water phase with the oil phase, and inject it into the chromatographic column to form a double continuous microemulsion, and let it stand; 4) After standing still, the double continuous microemulsion is aerobic at 50-80°C 5) heat-treat the dried product under aerobic conditions at 450-700°C; 6) pickle the heat-treated product; 7) modify the surface of the pickled product with silane to obtain SiO 2 Airgel monolithic columns. A kind of direct preparation SiO of the present invention 2 The airgel monolithic column method adopts normal pressure and low temperature, which can avoid the destruction of the monolithic column structure due to local severe vaporization during the drying process; the reaction temperature changes little, is easy to control, has a large specific surface area, high porosity, and requires relatively low working pressure. Small.

Description

Technical field [0001] The present invention belongs to the technical field of nano material is doped, particularly it relates to a direct preparation of SiO 2 Airgel monolithic column. Background technique [0002] Aerogels are aggregation of colloidal particles or molecules of another polymer network structure constituting the nanoporous, and filled with a gaseous dispersion medium is a highly dispersed solid material in the pores, and a solid phase are nanoscale pore structure, wet coagulation wherein in the drying process of the glue liquid component replaced with a gas while still maintaining its three-dimensional porous nanomaterial gel network. The resulting current porosity aerogels typically 80% to 99.8%, typically 50nm pore size within the range, the specific surface area can be up to l000m 2 / g. In addition, very low density airgel, and easy to be regulated by the process conditions. [0003] Continuous three-dimensional network structure in which the airgel such ther...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D15/20B01D15/22B01J20/286B01J20/30
CPCB01D15/206B01D15/22B01J20/286
Inventor 祝建中杨雪张欢陈靓范荣亮
Owner HOHAI UNIV