CN105174274A - Ambient preparation and control method of low-density SiO2 aerogel - Google Patents

Ambient preparation and control method of low-density SiO2 aerogel Download PDF

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CN105174274A
CN105174274A CN201510564122.8A CN201510564122A CN105174274A CN 105174274 A CN105174274 A CN 105174274A CN 201510564122 A CN201510564122 A CN 201510564122A CN 105174274 A CN105174274 A CN 105174274A
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sio
alcogel
aerogel
low density
control method
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吴会军
陈奇良
杨丽修
胡焕仪
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Guangzhou University
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Guangzhou University
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Abstract

The invention provides an ambient preparation and control method of low-density SiO2 aerogel. The method comprises the following steps of mixing silica sol prepared through acid catalysis and alkaline catalysis methods to prepare the SiO2 aerogel; aging the prepared SiO2 aerogel, testing compression modulus of the aged SiO2 aerogel, and stopping aging when the compression modulus of the aerogel achieves 0.25 to 2.5kPa; then carrying out one-step method surface modification and solvent replacement on the aged SiO2 aerogel to obtain modified SiO2 aerogel; using normal hexane to clean the modified SiO2 aerogel for many times, and ambient pressure drying at the temperature of 60 to 90 DEG C to respectively prepare the low-density SiO2 aerogel. The compression strength monitoring method is simple, so that the low-density SiO2 aerogel preparation process control is more feasible. The adopted ambient preparation method is low in cost and simple in process, and can be used for mass production.

Description

A kind of low density SiO 2the normal pressure of aerogel prepares control method
Technical field
The present invention relates to SiO 2the preparation field of aerogel, the normal pressure particularly relating to a kind of low density SiO2 aerogel prepares control method.
Background technology
SiO 2aerogel is a kind of amorphous nano solid material with spacial framework, there is ultra-low thermal conductivity (lower than synthermal lower to convected air), extremely-low density and the feature such as hydrophobic, have wide practical use in the field such as industry, building, space flight and aviation.But aerogel preparation technology needs supercritical drying usually, High Temperature High Pressure process cost is high and have certain risk, limits scale production and the large-scale application of aerogel.
For avoiding SiO 2high Temperature High Pressure supercritical drying in aerogel preparation process, need control sol-gel process parameter, and be aided with the processes such as aging ageing, surface modification and solvent exchange, to strengthen gel skeleton intensity or to improve aerogel hydrophobicity, aerogel is made to maintain nano-porous structure in constant pressure and dry process.Constant pressure and dry is prepared aerogel and is usually needed that sol-gel, ageing are aging, multiple processing step such as surface modification, solvent exchange, the processing parameter (as reaction times, pH value, reactant ratio, properties-correcting agent proportioning etc.) affecting aerogel performance is numerous, and is difficult to control SiO by the single or multiple processing parameter of research 2aerogel performance, uncontrollablely obtains low density SiO 2aerogel.
Current document focuses mostly at one or several processing parameter of sol-gel process to SiO 2the impact of aerogel performance, owing to influencing each other between multiple preparation technology parameter, explores low density SiO from multiple processing parameter combined influence 2aerogel preparation method controllability is particularly crucial, but still lacks feasible method at present.
Summary of the invention
The present invention proposes a kind of low density SiO 2the normal pressure of aerogel prepares control method, solves low density SiO 2the problem that aerogel preparation process affecting parameters is many, process control is difficult, the present invention proposes a kind of by alcogel modulus of compression state modulator SiO 2the method of aerogel density, is convenient to realize the hydrophobic SiO of low density 2the normal pressure preparation of aerogel and large-scale production application.
Technical scheme of the present invention is achieved in that a kind of low density SiO 2the normal pressure preparation of aerogel and control method, comprise following step:
Step one, acid catalysis:
Tetraethoxy is mixed with dehydrated alcohol, adds deionized water and hydrochloric acid and carry out acid catalyzed reaction and obtain silicon sol 1;
Step 2, base catalysis:
Base catalyzed reactions is carried out in the mixing of DMF, deionized water and ammoniacal liquor and obtains silicon sol 2;
Step 3, SiO 2prepared by alcogel:
Put into container after the silicon sol 2 that the silicon sol 1 step one obtained and step 2 obtain mixes, and leave standstill 0.5 ~ 48h, make SiO 2alcogel;
Step 4, SiO 2alcogel aging:
Alcogel step 3 obtained is put into ethanol and is carried out aging with quality than the mixed solution for 1:1 ~ 20, and gel skeleton is strengthened;
Step 5, SiO 2the modulus of compression test of alcogel:
Get the alcogel of different digestion time, and infiltrate alcogel outside surface with high boiling solvent, parcel, then tests its ultimate compression strength, and calculates SiO according to Hook's law 2the modulus of compression of alcogel, with modulus of compression monitoring SiO 2the frame strength of alcogel, when the modulus of compression of alcogel reaches 0.25 ~ 2.5kPa, stops aging;
Step 6, SiO 2the hydrophobically modified of alcogel and solvent exchange:
With the mixed solution of trimethylchlorosilane, dehydrated alcohol and normal hexane, by the SiO after aging 2alcogel carries out single stage method surface modification and solvent exchange, obtains the SiO of modification 2alcogel;
Step 7, constant pressure and dry:
With the SiO of normal hexane to modification 2alcogel repeatedly cleans, constant pressure and dry obtained low density SiO respectively at 60 ~ 90 DEG C 2aerogel.
Further, the mol ratio of described tetraethoxy, described dehydrated alcohol, described deionized water and described hydrochloric acid is 1:2 ~ 40:1 ~ 10:1 × 10 -5~ 1 × 10 -4.
Further, the mol ratio of described DMF, described deionized water and described ammoniacal liquor is 1 × 10 -4~ 1 × 10 -3: 1: 1 × 10 -3~ 5 × 10 -3.
Further, at test SiO 2before alcogel modulus of compression, first use glycerol and water mixed liquid to SiO 2alcogel sample infiltrates, and ftractures in test process to avoid it.
This by monitoring SiO 2low density SiO prepared by alcogel modulus of compression 2the control method of aerogel is simple, makes low density SiO 2process control prepared by aerogel is more feasible.
Further, mixed for the part in step 3 silicon sol 1 and silicon sol 2 are transferred in another container, and leave standstill 0.5 ~ 48h, obtain alcogel sample, the alcogel in step 5 takes from alcogel sample.
Further, the internal surface of the container in step 3 is smooth, and container is made up of plastics or rubber.
Further, the high boiling solvent described in step 5 is ethylene glycol, glycerol, one or more in dimethyl sulfoxide (DMSO).
Further, the low density SiO described in step 7 2the density of aerogel is less than 100kgm -3.
Beneficial effect of the present invention is:
1, low density SiO of the present invention 2the normal pressure of aerogel prepares control method by the skeleton strengthening process of Quantitative Monitoring alcogel in preparation process, with SiO 2alcogel modulus of compression is controling parameters, by controlling its modulus of compression in 0.25 ~ 2.5kPa scope, can prepare low density (as be less than 100kgm through follow-up constant pressure and dry etc. -3) SiO 2aerogel material, solves the problem that preparation process influence factor is many, control difficulty.
2, compressive strength monitoring method is simple, makes low density SiO 2process control prepared by aerogel is more feasible.
3, employing atmospheric preparation method cost is low, process simple, can be used for scale operation.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is a kind of low density SiO of the present invention 2the normal pressure of aerogel prepares the SiO of control method 2the SiO of alcogel 2the modulus of compression test process analysis chart of alcogel;
Fig. 2 is a kind of low density SiO of the present invention 2the normal pressure of aerogel prepares SiO in control method 2alcogel modulus of compression (X-coordinate) and the SiO prepared 2interact relation figure between aerogel density (ordinate zou);
Fig. 3 is a kind of low density SiO of the present invention 2the normal pressure of aerogel prepares the obtained low density SiO of control method 2the nanocrystailine microstructures of aerogel.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
A kind of low density SiO 2the normal pressure preparation of aerogel and control method, comprise following step:
Step one, acid catalysis:
Tetraethoxy is mixed with dehydrated alcohol, adds deionized water and hydrochloric acid and carry out acid catalyzed reaction and obtain silicon sol 1; The mol ratio of described tetraethoxy, described dehydrated alcohol, described deionized water and described hydrochloric acid is 1:2 ~ 40:1 ~ 10:1 × 10 -5~ 1 × 10 -4;
Step 2, base catalysis:
Base catalyzed reactions is carried out in the mixing of DMF, deionized water and ammoniacal liquor and obtains silicon sol 2; The mol ratio of described DMF, described deionized water and described ammoniacal liquor is 1 × 10 -4~ 1 × 10 -3: 1: 1 × 10 -3~ 5 × 10 -3;
Step 3, SiO 2prepared by alcogel:
Put into container after the silicon sol 2 that the silicon sol 1 step one obtained and step 2 obtain mixes, and leave standstill 0.5 ~ 48h, make SiO 2alcogel;
Step 4, SiO 2alcogel aging:
Alcogel step 3 obtained is put into ethanol and is carried out aging with quality than the mixed solution for 1:1 ~ 20, and gel skeleton is strengthened;
Step 5, SiO 2the modulus of compression test of alcogel:
Get the SiO of different digestion time 2alcogel, first uses glycerol and water mixed liquid to SiO 2alcogel sample infiltrates, and to avoid it to ftracture in test process, and infiltrates alcogel outside surface with high boiling solvent, and parcel, then tests its ultimate compression strength, and calculates SiO according to Hook's law 2the modulus of compression of alcogel, with modulus of compression monitoring SiO 2the frame strength of alcogel, when the modulus of compression of alcogel reaches 0.25 ~ 2.5kPa, stops aging; Described high boiling solvent is ethylene glycol, glycerol, one or more in dimethyl sulfoxide (DMSO);
According to SiO 2the intensity test curve of alcogel sample, calculates its modulus of compression (E) according to Hook's law:
E = 4 F Δ L πd 2 L ;
In formula, E is sample compression modulus, and F is pressure, and d is sample load face diameter, and L is length after sample deformations, and △ L is sample length variable quantity before and after test; According to modulus of compression monitoring SiO 2the frame strength of alcogel, controls low density SiO 2the preparation of aerogel;
Wherein Fig. 2 is SiO 2alcogel modulus of compression (X-coordinate) and the SiO prepared 2interact relation between aerogel density (ordinate zou), dash area represents by control SiO 2alcogel modulus of compression can prepare the SiO of density lower than 0.1g/cm3 at 0.25 ~ 2.5kPa 2aerogel.
Step 6, SiO 2the hydrophobically modified of alcogel and solvent exchange:
With the mixed solution of trimethylchlorosilane, dehydrated alcohol and normal hexane, by the SiO after aging 2alcogel carries out single stage method surface modification and solvent exchange, obtains the SiO of modification 2alcogel;
Step 7, constant pressure and dry:
With the SiO of normal hexane to modification 2alcogel repeatedly cleans, constant pressure and dry obtained low density SiO respectively at 60 ~ 90 DEG C 2aerogel; Described low density SiO 2the density of aerogel is less than 100kgm -3.
Low density SiO 2aerogel is a kind of amorphous nano solid material with spacial framework, has extremely-low density, ultra-low thermal conductivity, superelevation porosity and specific surface area, has wide practical use in the field such as industry, building, space flight and aviation, oxidation catalyst filter.
Wherein in Fig. 1, (a) is SiO 2state graph before the modulus of compression test of alcogel, (b) is SiO 2the state graph of the modulus of compression test beginning of alcogel, (c) is SiO 2state graph in the modulus of compression test of alcogel, (d) is SiO 2the state graph of the modulus of compression test end of alcogel.
Embodiment:
Density is 62kgm -3hydrophobic SiO 2the preparation control method of aerogel is as follows:
Step one, acid catalysis:
Mixed with dehydrated alcohol by tetraethoxy, add deionized water and hydrochloric acid carries out acid catalysis, the mol ratio controlling tetraethoxy, dehydrated alcohol, deionized water and hydrochloric acid is 1:7:1:10 -5; Be obtained by reacting silicon sol 1,
Step 2, base catalysis:
Base catalyzed reactions is carried out in the mixing of DMF, deionized water and ammoniacal liquor and obtains silicon sol 2; The mol ratio of described DMF, described deionized water and described ammoniacal liquor is 3 × 10 -4: 1:2 × 10 -3.
Step 3, SiO 2prepared by alcogel:
Put into container after the silicon sol 2 that the silicon sol 1 step one obtained and step 2 obtain mixes, and leave standstill 0.5 ~ 48h, make SiO 2alcogel;
Step 4, alcogel aging:
Alcogel step 3 obtained is put into ethanol and is carried out aging with quality than the mixed solution for 1:1 ~ 20, and gel skeleton is strengthened;
Step 5, SiO 2the modulus of compression test of alcogel:
Get the SiO of different digestion time 2alcogel, first uses glycerol and water mixed liquid to SiO 2alcogel sample infiltrates, and with high boiling solvent to SiO 2alcogel outside surface infiltrates, and parcel, then tests its ultimate compression strength, and calculates SiO according to Hook's law 2the modulus of compression of alcogel, with modulus of compression monitoring SiO 2the frame strength of alcogel, when the modulus of compression of alcogel reaches 0.5kPa, stops aging;
Step 6, SiO 2the hydrophobically modified of alcogel and solvent exchange:
With the mixed solution of trimethylchlorosilane, dehydrated alcohol and normal hexane, by the SiO after aging 2alcogel carries out single stage method surface modification and solvent exchange, obtains the SiO of modification 2alcogel;
Step 7, constant pressure and dry:
With the SiO of normal hexane to modification 2alcogel carries out twice cleaning, and at 60 DEG C, constant pressure and dry can obtain density for 12 hours is 62kgm -3siO 2aerogel.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.

Claims (8)

1. a low density SiO 2the normal pressure preparation of aerogel and control method, is characterized in that, comprise following step:
Step one, acid catalysis:
Tetraethoxy is mixed with dehydrated alcohol, adds deionized water and hydrochloric acid and carry out acid catalyzed reaction and obtain silicon sol 1;
Step 2, base catalysis:
Base catalyzed reactions is carried out in the mixing of DMF, deionized water and ammoniacal liquor and obtains silicon sol 2;
Step 3, SiO 2prepared by alcogel:
Put into container after the silicon sol 2 that the silicon sol 1 step one obtained and step 2 obtain mixes, and leave standstill 0.5 ~ 48h, make SiO 2alcogel;
Step 4, SiO 2alcogel aging:
Alcogel step 3 obtained is put into ethanol and is carried out aging with quality than the mixed solution for 1:1 ~ 20, and gel skeleton is strengthened;
Step 5, SiO 2the modulus of compression test of alcogel:
Get the alcogel of different digestion time, and infiltrate alcogel outside surface with high boiling solvent, parcel, then tests its ultimate compression strength, and calculates SiO according to Hook's law 2the modulus of compression of alcogel, with modulus of compression monitoring SiO 2the frame strength of alcogel, when the modulus of compression of alcogel reaches 0.25 ~ 2.5kPa, stops aging;
Step 6, SiO 2the hydrophobically modified of alcogel and solvent exchange:
With the mixed solution of trimethylchlorosilane, dehydrated alcohol and normal hexane, by the SiO after aging 2alcogel carries out single stage method surface modification and solvent exchange, obtains the SiO of modification 2alcogel;
Step 7, constant pressure and dry:
With the SiO of normal hexane to modification 2alcogel repeatedly cleans, constant pressure and dry obtained low density SiO respectively at 60 ~ 90 DEG C 2aerogel.
2. low density SiO according to claim 1 2the normal pressure of aerogel prepares control method, it is characterized in that: the mol ratio of described tetraethoxy, described dehydrated alcohol, described deionized water and described hydrochloric acid is 1:2 ~ 40:1 ~ 10:1 × 10 -5~ 1 × 10 -4.
3. low density SiO according to claim 1 2the normal pressure of aerogel prepares control method, it is characterized in that: the mol ratio of described DMF, described deionized water and described ammoniacal liquor is 1 × 10 -4~ 1 × 10 -3: 1: 1 × 10 -3~ 5 × 10 -3.
4. low density SiO according to claim 1 2the normal pressure of aerogel prepares control method, it is characterized in that: at test SiO 2before alcogel modulus of compression, first use glycerol and water mixed liquid to SiO 2alcogel sample infiltrates.
5. low density SiO according to claim 1 2the normal pressure of aerogel prepares control method, it is characterized in that: mixed for the part in step 3 silicon sol 1 and silicon sol 2 are transferred in another container, and leaves standstill 0.5 ~ 48h, and obtain alcogel sample, the alcogel in step 5 takes from alcogel sample.
6. low density SiO according to claim 1 2the normal pressure of aerogel prepares control method, it is characterized in that: the internal surface of the container in step 3 is smooth, and container is made up of plastics or rubber.
7. low density SiO according to claim 1 2the normal pressure of aerogel prepares control method, it is characterized in that: the high boiling solvent described in step 5 is ethylene glycol, glycerol, one or more in dimethyl sulfoxide (DMSO).
8. low density SiO according to claim 1 2the normal pressure of aerogel prepares control method, it is characterized in that: the low density SiO described in step 7 2the density of aerogel is less than 100kgm -3.
CN201510564122.8A 2015-09-06 2015-09-06 Ambient preparation and control method of low-density SiO2 aerogel Pending CN105174274A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105819457A (en) * 2016-03-14 2016-08-03 深圳中凝科技有限公司 Preparation method and applications of silica aerogel
CN106629752A (en) * 2016-12-01 2017-05-10 深圳中凝科技有限公司 Preparation method of elastic aerogel
CN106672985A (en) * 2017-01-04 2017-05-17 广东埃力生高新科技有限公司 Silicon dioxide aerogel with high specific surface area and fast preparation method thereof
CN110281593A (en) * 2019-06-23 2019-09-27 栗春侠 A kind of corrugated paper filler and preparation method thereof and corrugated paper
CN112850723A (en) * 2019-11-27 2021-05-28 台湾气凝胶科技材料开发股份有限公司 Preparation method of functional group modified aerogel particles for spinning and fiber spinning
CN113150365A (en) * 2021-05-27 2021-07-23 淮阴工学院 Preparation of melamine aerogel and fiber type clay reinforced melamine composite aerogel by normal pressure drying method
CN114620736A (en) * 2021-12-15 2022-06-14 航天海鹰(镇江)特种材料有限公司 Compression-controllable SiO2Aerogel composite material preparation method

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105819457A (en) * 2016-03-14 2016-08-03 深圳中凝科技有限公司 Preparation method and applications of silica aerogel
CN106629752A (en) * 2016-12-01 2017-05-10 深圳中凝科技有限公司 Preparation method of elastic aerogel
CN106672985A (en) * 2017-01-04 2017-05-17 广东埃力生高新科技有限公司 Silicon dioxide aerogel with high specific surface area and fast preparation method thereof
CN110281593A (en) * 2019-06-23 2019-09-27 栗春侠 A kind of corrugated paper filler and preparation method thereof and corrugated paper
CN112850723A (en) * 2019-11-27 2021-05-28 台湾气凝胶科技材料开发股份有限公司 Preparation method of functional group modified aerogel particles for spinning and fiber spinning
CN112850723B (en) * 2019-11-27 2022-11-04 台湾气凝胶科技材料开发股份有限公司 Preparation method of functional group modified aerogel particles for spinning and fiber spinning
CN113150365A (en) * 2021-05-27 2021-07-23 淮阴工学院 Preparation of melamine aerogel and fiber type clay reinforced melamine composite aerogel by normal pressure drying method
CN113150365B (en) * 2021-05-27 2023-01-13 淮阴工学院 Preparation of melamine aerogel and fiber type clay reinforced melamine composite aerogel by normal pressure drying method
CN114620736A (en) * 2021-12-15 2022-06-14 航天海鹰(镇江)特种材料有限公司 Compression-controllable SiO2Aerogel composite material preparation method

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