CN104609876A - Preparation method for low-density hydrophobic Al2O3 aerogel - Google Patents

Preparation method for low-density hydrophobic Al2O3 aerogel Download PDF

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CN104609876A
CN104609876A CN201510061634.2A CN201510061634A CN104609876A CN 104609876 A CN104609876 A CN 104609876A CN 201510061634 A CN201510061634 A CN 201510061634A CN 104609876 A CN104609876 A CN 104609876A
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solution
aerogel
wet gel
acetonitrile
al2o3
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CN104609876B (en
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任丽丽
李雪爱
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Southeast University
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Southeast University
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Abstract

The invention discloses a preparation method for low-density hydrophobic Al2O3 aerogel. The method comprises the following steps of adding ethyl alcohol into Al2O3 wet gel for liquid seal, standing for 5-72 hours at 25-60 DEG C, and removing ethyl alcohol; immersing the Al2O3 wet jel into an acetonitrile ethanol solution, standing for 5-72 hours at 25-60 DEG C, and removing the solution; at 25-60 DEG C, immersing the Al2O3 wet jel into a tetraethyl orthosilicate acetonitrile solution for 5-72 hours, removing the solution; then immersing the Al2O3 wet jel into an acetonitrile solution of trimethylchlorosilane for 5-72 hours, and then removing the solution, or, at 25-60 DEG C, immersing the Al2O3 wet jel into acetonitrile solution in which tetraethyl orthosilicate is mixed with trimethylchlorosilane for 5-72 hours, and removing the solution; soaking the Al2O3 wet jel with acetonitrile for 5-72 hours at 25-60 DEG C, and removing the solution; drying to obtain the Al2O3 aerogel. The method disclosed by the invention has the advantages that the operation is simple, the effect is remarkable, the aerogel density and shrinking percentage are greatly decreased, the hydrophilic surface of the aerogel is turned into a hydrophobic surface, and the application range of the aerogel is enlarged.

Description

A kind of low density hydrophobicity Al 2o 3the preparation method of aerogel
Technical field
The present invention relates to inorganic oxide preparation field, be specifically related to a kind of low density hydrophobicity Al 2o 3the preparation method of aerogel.
Background technology
Aerogel is a kind of nanoporous network structure of mutually assembling formation with ultramicron or high-polymer molecular, and in hole, be full of a kind of high dispersive solid material of gaseous state dispersion medium, its porosity high (80% ~ 99.8%), pore size distribution is at nanometer scale (1nm ~ 100nm).It is solid material the lightest in the world at present, and density can be low to moderate 0.002g/cm 3, being called " frost smoke " by people's image; Be the solid material that heat-proof quality is best in the world at present, room temperature in vacuo thermal conductivity can be low to moderate 0.001W/ (mK).In addition, also has much excellent characteristic, as low specific refraction, low perveance, low acoustic propagation velocity, in insulating refractory, catalyzer and support of the catalyst, silencing and damping material, novel high-energy particle detector, gas and water purification agent, special glass presoma etc., there is boundless application prospect.About the fundamental research of aerogel and applied research receive the extensive concern of Chinese scholars day by day, the aerogel application possessing unique excellent properties is more and more extensive, becomes the study hotspot in current Material Field.In numerous aerogel, Al 2o 3aerogel thermal conductivity low (30 DEG C, 1 normal atmosphere time heat-conduction coefficient be only 0.029W/ (mK), 400 DEG C, 1 normal atmosphere time heat-conduction coefficient be only 0.098W/ (mK), 800 DEG C, 1 normal atmosphere time heat-conduction coefficient be 0.298W/ (mK), be desirable high temperature insulating material.Due to Al 2o 3the high high-temp stability of aerogel is superior compared with aerosil, is paying close attention to widely as obtaining in high temperature insulating material and excellent catalyzer and support of the catalyst.Al 2o 3aerogel, because having superpower resistance to elevated temperatures (high temperature that ability is 2000 DEG C), efficiently catalytic performance and absorption property etc., becomes the splendid candidate material of lagging material, high temperature catalyst and carrier thereof.
But, the unprocessed alumina aerogels surface directly prepared is containing a large amount of hydrophilic hydroxy group, this makes their easy moisture absorptions in atmosphere, meet the water capacity easily broken, have impact on its performance such as sound, optical, electrical, thus limit the use occasion of aerogel, have impact on the application of aerogel in actual production life.Thus the wetting ability improving aerogel obtains the key that hydrophobic aerogel is the widespread use of promotion aerogel, is more and more subject to the attention of vast materialized scholar.
Summary of the invention
The present invention is intended to the Al prepared for present stage 2o 3its practical ranges of performance limitations such as aerogel surface hydrophilicity, propose a kind of employing two kinds of silylating reagents and carry out finishing to prepare low density hydrophobicity Al to the wet gel in weathering process 2o 3the method of aerogel.
The present invention is by the following technical solutions:
A kind of low density hydrophobicity Al 2o 3the preparation method of aerogel, adopts two kinds of silylating reagents to carry out finishing to the wet gel in weathering process, comprises the steps:
Step one, employing sol-gel method prepare Al 2o 3wet gel;
Step 2, the Al prepared to step one 2o 3add ethanol in wet gel and carry out fluid-tight, at 25 ~ 60 DEG C, aging 5 ~ 72h, removes ethanol afterwards;
Step 3, the Al that step 2 is prepared 2o 3wet gel immerses in acetonitrile ethanolic soln, carries out solvent replacing 5 ~ 72h, remove solution afterwards at 25 ~ 60 DEG C; At 25 ~ 60 DEG C, by Al 2o 3wet gel immerses in the acetonitrile solution of tetraethyl orthosilicate (TEOS) and carries out finishing 5 ~ 72h, removes solution, then by Al 2o 3wet gel immerses in the acetonitrile solution of trimethylchlorosilane (TMCS) and carries out finishing 5 ~ 72h, removes solution or at 25 ~ 60 DEG C, by Al 2o 3wet gel immerses in the acetonitrile solution of TEOS and TMCS mixing and carries out finishing 5 ~ 72h, removes solution; Afterwards by Al 2o 3wet gel soaks 5 ~ 72h with acetonitrile at 25 ~ 60 DEG C, removes solution;
Step 4, the Al that step 3 is modified 2o 3wet gel is dry, obtains Al 2o 3aerogel.
Described in step 3, the concentration of acetonitrile ethanolic soln is more than 30v/v%; The concentration of the acetonitrile solution of described TEOS is 30v/v% ~ 80v/v%; The concentration of the acetonitrile solution of described TMCS is 1v/v% ~ 2v/v%; In the acetonitrile solution of described TEOS and TMCS mixing, the concentration of tetraethyl orthosilicate is 30v/v% ~ 80v/v%, and the concentration of trimethylchlorosilane is 1v/v% ~ 2v/v%.
Drying means described in step 4 comprises supercritical drying, constant pressure and dry or organic solvent sublimation drying.
Beneficial effect of the present invention:
Low density hydrophobicity Al provided by the invention 2o 3the preparation method of aerogel, adopt two kinds of silylating reagents to carry out finishing to the wet gel in weathering process, simple to operate, successful, the aerogel of contrast unmodified, aerogel density and shrinking percentage significantly reduce, and make the hydrophilic surface of aerogel become water repellent surface, expand the range of application of aerogel.
Accompanying drawing explanation
Fig. 1 is the aerogel that embodiment 1 (right side) and comparative example 1 (left side) are prepared.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention done and further explain.The following example only for illustration of the present invention, but is not used for limiting practical range of the present invention.
A kind of low density hydrophobicity Al 2o 3the preparation method of aerogel, adopts two kinds of silylating reagents to carry out finishing to the wet gel in weathering process, comprises the steps:
Step one, employing sol-gel method prepare Al 2o 3wet gel;
Step 2, the Al prepared to step one 2o 3add ethanol in wet gel and carry out fluid-tight, at 25 ~ 60 DEG C, aging 5 ~ 72h, removes ethanol afterwards;
Step 3, the Al that step 2 is prepared 2o 3wet gel immerses in the acetonitrile ethanolic soln of more than 30v/v%, carries out solvent replacing 5 ~ 72h, remove solution afterwards at 25 ~ 60 DEG C; At 25 ~ 60 DEG C, by Al 2o 3wet gel immerses in the acetonitrile solution of 30v/v% ~ 80v/v%TEOS and carries out finishing 5 ~ 72h, removes solution, then by Al 2o 3wet gel immerses in the acetonitrile solution of 1v/v% ~ 2v/v%TMCS and carries out finishing 5 ~ 72h, removes solution or at 25 ~ 60 DEG C, by Al 2o 3wet gel immerses in the acetonitrile solution of TEOS and TMCS mixing and carries out finishing 5 ~ 72h, removes solution; Afterwards by Al 2o 3wet gel soaks 5 ~ 72h with acetonitrile at 25 ~ 60 DEG C, removes solution; Wherein, in the acetonitrile solution of described TEOS and TMCS mixing, the concentration of TEOS is the concentration of 30v/v% ~ 80v/v%, TMCS is 1v/v% ~ 2v/v%;
Step 4, the Al that step 3 is modified 2o 3wet gel adopts the methods such as supercritical drying, constant pressure and dry or organic solvent sublimation drying dry, obtains Al 2o 3aerogel.
Sol-gel method is adopted to prepare Al in following examples 2o 3the concrete steps of wet gel are as follows:
24mL water and 56mL ethanol are joined in there-necked flask, mix, when oil bath is warming up to 80 DEG C, add the 1mol/L hydrochloric acid of 24.143g Aluminium chloride hexahydrate and 10mL, return stirring 4h, after being cooled to room temperature, dripping 56mL propylene oxide in ice-water bath, mix, dividing in small beaker afterwards by the uniform liquid in there-necked flask, 15mL in each beaker, then puts into 40 DEG C of environment and leaves standstill by beaker, treat that the beaker 45 ° of liquid that tilt no longer flow and namely form wet gel.
Embodiment 1 (first TEOS modifies, and then TMCS modifies)
1, to Al prepared by above-mentioned employing sol-gel method 2o 3add a small amount of ethanol in wet gel and seal wet gel surface, aging 24h at 40 DEG C, removes ethanol wherein afterwards.
2, the acetonitrile ethanolic soln adding 50v/v% did not have wet gel, carries out solvent replacing 24h, remove solution afterwards at 40 DEG C; At 40 DEG C, the acetonitrile solution adding 50v/v%TEOS did not have wet gel, and finishing 24h, removes solution, then the acetonitrile solution adding 1.85v/v%TMCS did not have wet gel, and finishing 24h, removes solution; At 40 DEG C, add acetonitrile and do not have wet gel, soak 24h, afterwards solution is removed.
3, dry by organic solvent sublimation drying method, wherein organic solvent adopts acetonitrile, and vacuum tightness is 80 ~ 90kp, and temperature is 50 DEG C, and time of drying is 24h, obtains the Al after modifying 2o 3aerogel.
Embodiment 2 (TEOS+TMCS modifies simultaneously)
1, to Al prepared by above-mentioned employing sol-gel method 2o 3add a small amount of ethanol in wet gel and seal wet gel surface, aging 24h at 40 DEG C, removes ethanol wherein afterwards.
2, the acetonitrile ethanolic soln adding 50v/v% did not have wet gel, carries out solvent replacing 24h, remove solution afterwards at 40 DEG C; At 40 DEG C, the acetonitrile solution (wherein the concentration of TEOS is the concentration of 50v/v%, TMCS is 1.85v/v%) adding TEOS and TMCS mixing did not have wet gel, and finishing 24h, removes solution; At 40 DEG C, add acetonitrile and do not have wet gel, soak 24h, afterwards solution is removed.
3, carry out drying by the method that same embodiment 1 is identical, obtain the Al after modifying 2o 3aerogel.
Comparative example 1 (unmodified)
1, to Al prepared by above-mentioned employing sol-gel method 2o 3add a small amount of ethanol in wet gel and seal wet gel surface, aging 24h at 40 DEG C, removes ethanol wherein afterwards.
2, the acetonitrile ethanolic soln adding 30v/v% did not have wet gel, carries out solvent replacing 24h, remove solution afterwards at 40 DEG C; At 40 DEG C, the acetonitrile ethanolic soln adding 50v/v% did not have wet gel, soaked 24h, removed solution; At 40 DEG C, add acetonitrile and do not have wet gel, soak 24h, afterwards solution is removed.
3, carry out drying by the method that same embodiment 1 is identical, obtain the Al after modifying 2o 3aerogel.
Comparative example 2 (TMCS modification)
1, to Al prepared by above-mentioned employing sol-gel method 2o 3add a small amount of ethanol in wet gel and seal wet gel surface, aging 24h at 40 DEG C, removes ethanol wherein afterwards.
2, the acetonitrile ethanolic soln adding 50v/v% did not have wet gel, carries out solvent replacing 24h, remove solution afterwards at 40 DEG C; The acetonitrile solution adding the TMCS of 1.85v/v% did not have wet gel, and finishing 24h, removes solution; At 40 DEG C, add acetonitrile and do not have wet gel, soak 24h, afterwards solution is removed.
3, carry out drying by the method that same embodiment 1 is identical, obtain the Al after modifying 2o 3aerogel.
Comparative example 3 (TEOS modification)
1, to Al prepared by above-mentioned employing sol-gel method 2o 3add a small amount of ethanol in wet gel and seal wet gel surface, aging 24h at 40 DEG C, removes ethanol wherein afterwards.
2, the acetonitrile ethanolic soln adding 50v/v% did not have wet gel, carries out solvent replacing 24h, remove solution afterwards at 40 DEG C; The acetonitrile solution adding the TEOS of 50v/v% did not have wet gel, and finishing 24h, removes solution; At 40 DEG C, add acetonitrile and do not have wet gel, soak 24h, afterwards solution is removed.
3, carry out drying by the method that same embodiment 1 is identical, obtain the Al after modifying 2o 3aerogel.
Comparative example 4 (first TMCS modifies, and then TEOS modifies)
1, to Al prepared by above-mentioned employing sol-gel method 2o 3add a small amount of ethanol in wet gel and seal wet gel surface, aging 24h at 40 DEG C, removes ethanol wherein afterwards.
2, the acetonitrile ethanolic soln adding 50v/v% did not have wet gel, carries out solvent replacing 24h, remove solution afterwards at 40 DEG C; At 40 DEG C, the acetonitrile solution adding the TMCS of 1.85v/v% did not have wet gel, and finishing 24h, removes solution, then the acetonitrile solution of the TEOS adding 50v/v% did not have wet gel finishing 24h, removed solution; At 40 DEG C, add acetonitrile and do not have wet gel, soak 24h, afterwards solution is removed.
3, carry out drying by the method that same embodiment 1 is identical, obtain the Al after modifying 2o 3aerogel.
The aerogel that embodiment 1 (right side) and comparative example 1 (left side) are prepared as shown in Figure 1, in aging and drying process, wet gel can slowly shrink to such an extent as to volume can diminish, contrast two figure and can find out that first TEOS modifies, the aerogel volume that rear TMCS modifies is large, that namely shrinks is little, and the density of rough calculation aerogel is by 0.933g/cm 3be reduced to 0.502g/cm 3, shrinking percentage is reduced to 60.8% by 91.8%, describes TEOS and TMCS as coating materials for the preparation of low density hydrophobicity Al 2o 3the guess of aerogel is feasible, and successful.First modify high by the circulation ratio of TMCS modification with TEOS, the amplitude that contraction diminishes is large, best results again; The effect of modifying after TEOS and TMCS mixing is taken second place; First modify again with the aerogel surface peeling that TEOS modifies with TMCS, aerogel bulk degree is bad; And be used alone TEOS modify surface also peeling, block degree is bad, effect be similar to first with TMCS modify again with TEOS modify; The aerogel being used alone TMCS modification shrinks large, and the aerogel density prepared is large, similar with the effect of unmodified.

Claims (4)

1. a low density hydrophobicity Al 2o 3the preparation method of aerogel, is characterized in that, adopts two kinds of silylating reagents to carry out finishing to the wet gel in weathering process, comprises the steps:
Step one, employing sol-gel method prepare Al 2o 3wet gel;
Step 2, the Al prepared to step one 2o 3add ethanol in wet gel and carry out fluid-tight, at 25 ~ 60 DEG C, aging 5 ~ 72h, removes ethanol afterwards;
Step 3, the Al that step 2 is prepared 2o 3wet gel immerses in acetonitrile ethanolic soln, carries out solvent replacing 5 ~ 72h, remove solution afterwards at 25 ~ 60 DEG C; At 25 ~ 60 DEG C, by Al 2o 3wet gel immerses in the acetonitrile solution of tetraethyl orthosilicate and carries out finishing 5 ~ 72h, removes solution, then by Al 2o 3wet gel immerses in the acetonitrile solution of trimethylchlorosilane and carries out finishing 5 ~ 72h, removes solution or at 25 ~ 60 DEG C, by Al 2o 3wet gel immerses in the acetonitrile solution of tetraethyl orthosilicate and trimethylchlorosilane mixing and carries out finishing 5 ~ 72h, removes solution; Afterwards by Al 2o 3wet gel soaks 5 ~ 72h with acetonitrile at 25 ~ 60 DEG C, removes solution;
Step 4, the Al that step 3 is modified 2o 3wet gel is dry, obtains the Al after modifying 2o 3aerogel.
2. low density hydrophobicity Al according to claim 1 2o 3the preparation method of aerogel, is characterized in that, described in step 3, the concentration of acetonitrile ethanolic soln is more than 30v/v%.
3. low density hydrophobicity Al according to claim 1 2o 3the preparation method of aerogel, is characterized in that, the concentration of the acetonitrile solution of step 3 tetraethyl orthosilicate used is 30v/v% ~ 80v/v%; The concentration of the acetonitrile solution of described trimethylchlorosilane is 1v/v% ~ 2v/v%; In the acetonitrile solution of described tetraethyl orthosilicate and trimethylchlorosilane mixing, the concentration of tetraethyl orthosilicate is 30v/v% ~ 80v/v%, and the concentration of trimethylchlorosilane is 1v/v% ~ 2v/v%.
4. low density hydrophobicity Al according to claim 1 2o 3the preparation method of aerogel, is characterized in that, drying described in step 4 comprises supercritical drying, constant pressure and dry or organic solvent sublimation drying.
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CN115504493A (en) * 2022-11-07 2022-12-23 神华准能资源综合开发有限公司 Method for preparing alumina aerogel from crystalline aluminum chloride

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CN115504493A (en) * 2022-11-07 2022-12-23 神华准能资源综合开发有限公司 Method for preparing alumina aerogel from crystalline aluminum chloride
CN115504493B (en) * 2022-11-07 2023-11-28 神华准能资源综合开发有限公司 Method for preparing alumina aerogel from crystallized aluminum chloride

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