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Recycling methods of normal hexane in silica-based aerogel preparation process

A preparation process, n-hexane technology, applied in the direction of silicon oxide, silicon dioxide, absorption purification/separation, etc., can solve the problems of recovery that have not been reported yet, reduce the cost of normal pressure preparation, increase the utilization rate, and the operation method is simple and easy line effect

Inactive Publication Date: 2012-09-19
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] So far, it has not been reported that the use of aqueous phase extraction and anhydrous calcium chloride method to recover n-hexane mixed with ethanol

Method used

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  • Recycling methods of normal hexane in silica-based aerogel preparation process

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Embodiment 1

[0022] Embodiment 1 aqueous phase extraction method

[0023] The aqueous phase extraction method uses the principle of the difference in mutual solubility of liquids to separate n-hexane. Ethanol and water are miscible in any ratio, but n-hexane is insoluble in water. Therefore, the aqueous phase extraction method can be used to purify n-hexane. The experimental method is as follows: take 20mL of recovered mother liquor in a beaker, add 20mL of deionized water to it twice, shake and leave it for half an hour, and take the upper layer liquid after liquid separation, namely It is purified n-hexane. The composition and purity of the upper liquid were analyzed by gas chromatography and refractometer. Wherein the analysis condition of gas chromatography is column temperature 34 ℃, detector: 170 ℃, vaporization chamber: 120 ℃, H 2 Flow 30mL / min, air flow 400mL / min, N 2 The flow rate is 25mL / min. Gas phase data show that the purity of n-hexane purified by aqueous phase ...

Embodiment 2

[0024] Embodiment 2 anhydrous calcium chloride method

[0025] The anhydrous calcium chloride method utilizes chemical reactions:

[0026]

[0027] Ethanol can react with anhydrous calcium chloride at room temperature to form a complex, which can exist stably at room temperature, while n-hexane does not react with calcium chloride. The experimental method is as follows: take 3g of anhydrous calcium chloride and add it to 20mL of recovered mother liquor, vibrate, stand still, filter, and collect the filtrate, which is purified n-hexane. The filtrate composition and purity were analyzed by gas chromatography and refractive index. Wherein the analysis condition of gas chromatography is column temperature 34 ℃, detector: 170 ℃, vaporization chamber: 120 ℃, H 2 Flow 30mL / min, air flow 400mL / min, N 2 The flow rate is 25mL / min, and the gas phase data show that the purity of n-hexane purified by anhydrous calcium chloride method reaches 99%, and the refractive index mea...

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Abstract

The invention provides recycling methods of normal hexane in a silica-based aerogel preparation process and belongs to the technical field of novel material preparation. A water-phase extraction method is that ethanol in the normal hexane is removed by utilizing deionized water, the normal hexane is purified, a certain amount of deionized water is added in recovered normal hexane mother solution, and the solution is oscillated, stood and separated. An anhydrous calcium chloride method is that the normal hexane is purified by utilizing the principle that reaction of the ethanol and anhydrous calcium chloride can generate a stable complex at normal temperature, a certain amount of anhydrous calcium chloride is added in the recovered normal hexane mother solution, the solution is oscillated, stood, filtered and separated, and the purity of the recovered normal hexane is detected under the same gaseous phase condition. The purity of the normal hexane purified by the two methods reaches above 99%, the normal hexane can be recycled in the silica-based aerogel preparation process, and further preparation cost of silica-based aerogel is reduced. The two methods have the advantages of being easy in reaction control, simple in technical process, low in cost and the like.

Description

technical field [0001] The invention belongs to the technical field of new material preparation, and relates to two recycling methods of n-hexane in the preparation process of silicon-based airgel, in particular to a method for recycling n-hexane by using an aqueous phase extraction method and an anhydrous calcium chloride method , so as to achieve the purpose of controlling the cost of airgel preparation, and promote the faster industrialization of airgel. Background technique [0002] SiO 2 Airgel is a lightweight nanoporous amorphous solid material with many excellent properties, such as high porosity (~99%), low density (~0.3g / cm 3 ), large specific surface area (1600m 2 / g), low thermal conductivity (<0.02W / mK), low sound velocity (~100m / s), low refractive index (1.01-1.10), etc. Therefore SiO 2 Aerogels have broad application prospects in the fields of thermal insulation materials, acoustic impedance coupling materials, rocket liquid propellant storage media, C...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C9/15C07C7/10C07C7/11C01B33/16
Inventor 陈敏吴寅寅朱建军姜德立谢吉民孟素慈潘艾霞
Owner JIANGSU UNIV
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