CN103435055A - Method for preparing low density silica aerogel under normal pressure - Google Patents

Method for preparing low density silica aerogel under normal pressure Download PDF

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CN103435055A
CN103435055A CN2013102727158A CN201310272715A CN103435055A CN 103435055 A CN103435055 A CN 103435055A CN 2013102727158 A CN2013102727158 A CN 2013102727158A CN 201310272715 A CN201310272715 A CN 201310272715A CN 103435055 A CN103435055 A CN 103435055A
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acid
normal hexane
density
aerogel
trimethylchlorosilane
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尉明全
张波
张闯
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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Abstract

The present invention discloses a method for preparing low density silica aerogel under normal pressure. The method comprises: mixing tetraethoxysilane, water and ethanol according to a volume ratio of 1:0.5-19:1-29, adding an acid to adjust the pH value to 3-4, carrying out catalysis hydrolysis, adding an alkali to adjust the pH value to 6-6.5, carrying out catalysis gelating for 8-10 min to obtain a wet gel, aging the wet gel for 6-36 h at a room temperature, adding n-hexane to carry out solvent replacement for 6-36 h, immersing in a trimethylchlorosilane and n-hexane mixed solution to carry out hydrophobic modification for 12-15 h, adopting a n-hexane washing solution to remove the modification solution, placing into a muffle furnace to heat to a temperature of 30-250 DEG C, drying, and finally cooling to a room temperature to obtain the silica aerogel. Test results show that the density of the SiO2 aerogel is 50-80 kg/m<3> and is significantly lower than the density of the SiO2 aerogel prepared under the normal pressure dry condition in most of the public reports.

Description

A kind of method for preparing low-density silicon dioxide aerogel under normal pressure
(1) technical field
The present invention relates to the preparation of aerosil, especially relate to preparation low density SiO under the constant pressure and dry condition 2the method of aerogel.
(2) background technology
Aerogel is the nano-meter porous amorphous solid material of a kind of lightweight formed by the colloidal particle polycondensation, has continuous network structure, has the homogeneity of nanoscale on microcosmic, and its aperture and whole particle are nano level.Thisly take solid-phase and the pore texture that gas is dispersion medium and make it there are unique physicochemical property.And density on its physicochemical property impact significantly, the lower porosity of density is higher, specific surface area is larger, specific refractory power is lower, thermal conductivity is lower etc.The aerogel application is very extensive, in fields such as heat-insulation and heat-preservation, Industrial Catalysis, aerospace, medicine chemical industry, all has broad application prospects.
Prepare at present low density SiO 2aerogel generally adopts the supercritical drying mode, and its principle is: under supercritical state, between gas and liquid, there will be no interface to exist, but become a kind of uniform fluid between gas-liquid.Replaced out the time in colloid when this fluid, because there not being liquid-gas interface, thereby there do not is wicking action, therefore just can not cause the contraction of colloid or cave in, finally obtain having the low density aerogel of nanostructure.The Chinese patent that for example publication number is CN102602943A, take organosilicon as the silicon source, adopt single stage method to prepare aerosil, what the drying process of aerogel adopted is the supercritical drying drying method, service temperature is that 290 ℃, pressure are 23.5MPa, and the density of aerogel is 30kg/m 3.The shortcoming of supercritical drying is to need High Temperature High Pressure in process, makes operation more dangerous, and has increased the production cost of aerogel.The Chinese patent that publication number is 102317209A, take tetraethoxy as the silicon source, ethanol is solvent, mixture is stirred to 1h under 70 ℃ of conditions, make its gel, aging under condition of normal pressure by regulating pH value, wherein gel time is 10～47s, take hexamethyldisilazane as surface-modifying agent, finally carry out supercritical drying.The density that finally makes the aerogel sample is 140～360kg/m 3.This method complicated process of preparation, condition is difficult to control, and product density is larger.Publication number is 1724353 patents from Tsing-Hua University, take rice hull ash as raw material, by the leaching of inorganic strong alkali, the neutralization of organic acid, after aging, washing, organic solvent displacement, finishing, supercritical drying, make white aerosil sample, its density is at 39.8～45.2kg/m 3between.In the method, acid-base waste fluid is many, and environmental pollution is larger.
Although supercritical drying can access quality low density SiO preferably 2aerogel, but because of its complex process, preparation cost is high, the operation environment safety coefficient is low etc., and factor has seriously restricted its large-scale production.And adopt constant pressure and dry technique to prepare low density SiO 2aerogel can significantly reduce preparation cost, more is conducive to suitability for industrialized production.Therefore, research and development low density SiO 2the constant pressure and dry preparation method of aerogel is extremely important, and has been one of focus of aerogel research field.The open report of this respect is a lot of at present.For example publication number is 101264891 patents from University of Science & Technology, Beijing, take methyl silicate and tetraethoxy as the silicon source, ethanol is solvent, sulphur acid for adjusting pH value by 0.35mol/L, bathe heating 1.5h hydrolysis at 80 ℃ of Water Unders, then add ammoniacal liquor to make its gel, soak 36h in dehydrated alcohol after, put into the aging 8d of pressure pan of the mixture that tetraethoxy, ethanol, water are housed, obtain the aerogel sample through the normal temperature drying again, density is 170～260kg/m 3.This invents not only complex process, digestion time is long, and the aerogel sample rate of gained is very large.Publication number is the patent of 102020285A from Shenzhen University, take service water glass as the silicon source, obtain wet gel by single stage method, use again soaked in absolute ethyl alcohol, washing, modifying agent is trimethylchlorosilane, after hydrophobically modified, with normal hexane, wash for several times again, the standing aerogel sample that obtains of room temperature, its density is 0.1～0.18g/cm 3, i.e. 100～180kg/m 3.This scheme ethanol usage quantity is large, is difficult to reclaim, and product density is also higher.The people such as the Wang Dongdong of Sinosteel Corporation take silicon sol as raw material, hydrochloric acid be catalyzer, regulate the pH value and make its gel, aging in the mixed solution of ethanol and ethanol and tetraethoxy, do not carry out solvent exchange and hydrophobically modified, the product density finally obtained is 140～400kg/m 3.The method preparation cycle is long, complicated operation, and product density is obviously higher.It is presoma that the people such as the Li Hua of Inner Mongol University of Technology adopt tetraethoxy, ethanol is solvent, with soda acid two-step catalysis, gel, after gel formation, with normal hexane, carries out solvent exchange, carry out again the silanization hydrophobically modified, finally from 30～70 ℃ of temperature programming dryings.Although this method technique is simple, the production cycle is long, and product density is higher, is about 70～200kg/m 3.Publication number is 101691227 patents from Xiamen University, take tetraethoxy as presoma, ethanol be solvent, form gel by the soda acid two-step catalysis, then through aging, hydrophobically modified, washing, through the temperature programming drying, obtain the aerogel sample, gained density is 170kg/m 3.Solvent exchange is not carried out in this invention, gained SiO 2aerogel density is higher.The Chinese patent that publication number is CN102897779A be take water glass as the silicon source, adopts two-step approach--acid-catalyzed hydrolysis, base catalysis gel, last adjust pH to 8.0 left and right.After the sample gel, use dehydrated alcohol to strengthen network skeleton structure and solvent replacing, the mixing solutions that hydrophobically modified reagent is trimethylchlorosilane, dehydrated alcohol and normal hexane, temperature programming to 200 ℃ dry 6h after washing.The method complicated operation, aging and drying temperature is high to equipment requirements, last products obtained therefrom density is 110～240kg/m 3.
At present, although constant pressure and dry technique has the advantages such as pair equipment requirements is simple, security good, productive expense is low, the general shortcoming such as higher of long, product density of production cycle is also arranged.
(3) summary of the invention
, operational hazards high for the equipment cost in the supercritical drying drying process, energy consumption are large, and the large and longer problem and shortage of production cycle of product density in constant pressure and dry technique, the present invention passes through Optimizing Technical, the ratio, shortening wet gel digestion time, solvent exchange time and the improvement drying step that change silicon source and dehydrated alcohol and water operate to shorten the production cycle and reduce product density, develop quick preparation low density SiO under a kind of condition of normal pressure 2the method of aerogel, its minimum 49kg/m that reaches 3.
The object of the present invention is to provide a kind of low density SiO for preparing fast under the constant pressure and dry condition 2the method of aerogel, the method technique is simple, with short production cycle, productive rate is high, product density is low, is easy to large-scale industrial production.
For achieving the above object, the present invention adopts following technical proposals:
A kind of method for preparing low-density silicon dioxide aerogel under normal pressure, described method comprises the steps:
By tetraethoxy, water and ethanol are that the ratio of 1:0.5～19:1～29 is mixed by volume, adding sour adjust pH is 3～4, catalytic hydrolysis 30～40 minutes, obtain silicon sol, adding the adjusting PH with base value is 6～6.5 again, catalysis gel 8～10 minutes, obtain wet gel, by wet gel aging 6～36h at room temperature, add normal hexane to carry out solvent exchange 6～36h, gel after displacement is immersed in the mixing solutions of trimethylchlorosilane and normal hexane and carries out hydrophobically modified 12～15 hours, then remove modification liquid with the normal hexane washing, put into again retort furnace and be warming up to 30～250 ℃ of dryings, last cool to room temperature makes aerosil, described acid is mineral acid, monobasic organic acid or binary organic acid, described alkali is mineral alkali, in the mixing solutions of described trimethylchlorosilane and normal hexane, the volume ratio of trimethylchlorosilane and normal hexane is 1～50:100.
The volume ratio of described tetraethoxy, water and ethanol is preferably 1:0.5～4:1～9, more preferably 1:0.5～3:1～7.
Described acid is preferably formic acid, nitric acid, phenylformic acid, hydrochloric acid or acetic acid, is preferably nitric acid.
Described alkali is preferably potassium hydroxide, sodium hydroxide or ammoniacal liquor, preferably potassium hydroxide or sodium hydroxide.
In the mixing solutions of described trimethylchlorosilane and normal hexane, the volume ratio of trimethylchlorosilane and normal hexane is preferably 5～35:100.
The temperature of described drying is preferably 50～150 ℃, more preferably 100～150 ℃.
The time of described drying is generally 2～3 hours.
The volumetric usage of the normal hexane for solvent exchange of the present invention is generally 10～15 times of volume of tetraethoxy.
The volumetric usage of the mixing solutions of described trimethylchlorosilane and normal hexane is generally 10～15 times of volume of tetraethoxy.
The aging time of the present invention is 6～24h, preferably 12～18h preferably.
The time of described solvent exchange is 6～24h preferably, preferably 12～18h.
Beneficial effect of the present invention is:
1, the present invention adopts sol-gel technique to synthesize low density SiO 2the aerogel nano material, the production cycle obviously shortens, and has improved production efficiency, has saved the energy.
2, reaction conditions of the present invention is simple, controlled, and the silicon source is fast in acid catalysis Water Under solution speed, and under the base catalysis condition, gel time is short, and about 8min can form gel, so just shortens the preparation time of gel.
3, the SiO that the present invention obtains 2aerogel, show after tested, and its density is at 50～80kg/m 3between, be starkly lower than the SiO prepared under the constant pressure and dry condition of the open report of great majority 2the density of aerogel.
(4) embodiment
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited to this.
Embodiment 1～5: different tetraethoxys, water, ethanol volume ratio are to SiO 2the impact of aerogel density
Get tetraethoxy 4mL, according to different volumes ratio water intaking in table 1, dehydrated alcohol, by tetraethoxy, water and dehydrated alcohol mixing and stirring, add 1mol/L nitric acid adjust pH to 3.5, obtain silicon sol after being hydrolyzed 30 minutes.Add while stirring 1mol/L sodium hydroxide solution adjust pH to 6.5, the catalysis gel obtains wet gel in 8 minutes, by wet gel aging 18h at room temperature, carry out solvent exchange 18h with the 40mL normal hexane again, gel sample after displacement is immersed in V (trimethylchlorosilane (TMCS)): V (normal hexane) for hydrophobically modified in the mixing solutions 40mL of 10:100 12 hours, remove modification liquid 2 times with the washing of 20mL normal hexane, put into the retort furnace Program and be warming up to 200 ℃ of dry 2h, last cool to room temperature obtains SiO 2aerogel.The sample of gained is crossed to 200 mesh sieve, with balance weigh quality, graduated cylinder measures volume, the ratio of the two can obtain the density of aerogel.The volume ratio of embodiment 1 tetraethoxy, water and ethanol is 1:0.5:1, the volume ratio of embodiment 2 tetraethoxys, water and ethanol is 1:1:3, the volume ratio of embodiment 3 tetraethoxys, water and ethanol is 1:2:5, the volume ratio of embodiment 4 tetraethoxys, water and ethanol is 1:3:7, and the volume ratio of embodiment 5 tetraethoxys, water and ethanol is 1:4:9.The results are shown in Table 1.
The different tetraethoxys of table 1 embodiment 1～5 (TEOS), water, ethanol volume ratio are to SiO 2the impact of aerogel density
Embodiment V(TEOS):V(H 2O):V(EtOH) Density (kg/m 3）
1 1:0.5:1 58
2 1:1:3 71
3 1:2:5 77
4 1:3:7 78
5 1:4:9 80
Embodiment 6～10: different acid catalysts are to SiO 2the impact of aerogel density
According to the method for embodiment 1, get tetraethoxy 4mL, by V (TEOS): V (H 2o): V (EtOH) stirs for the mixing solutions of 1:0.5:1, difference is, carry out catalytic hydrolysis after adding different acid to adjust pH to 3.5, the acid added is as shown in table 1, add again 1mol/L potassium hydroxide solution adjust pH to 6.5, the catalysis gel obtains wet gel in 8 minutes, by wet gel aging 18h at room temperature, follow-up other operations are with embodiment 1, wherein embodiment 6 acid catalyst used is formic acid, embodiment 7 acid catalyst used is 1mol/L nitric acid, embodiment 8 acid catalyst used is phenylformic acid, embodiment 9 acid used is 1mol/L hydrochloric acid, embodiment 10 acid used is acetic acid.The results are shown in Table 2.
The different acid catalysts of table 2 are to SiO 2the impact of aerogel density
Embodiment Acid catalyst Density (kg/m 3）
[0034]?
6 Formic acid 63
7 1mol/L nitric acid 67
8 Phenylformic acid 76
9 1mol/L hydrochloric acid 68
10 Acetic acid 66
Embodiment 11～13: the Different Alkali catalyzer is to SiO 2the impact of aerogel density
According to the method for embodiment 2, get tetraethoxy 4mL, adopt V (TEOS): V (H 2o): the mixing solutions that V (EtOH) is 1:1:3, other operations are with embodiment 2, difference is to add different adjusting PH with base values to 6.5 after catalytic hydrolysis, carry out the catalysis gel, as shown in table 3, embodiment 11 is 1mol/L potassium hydroxide solutions, and embodiment 12 is 0.5mol/L sodium hydroxide solutions, and embodiment 13 is 1mol/L ammoniacal liquor.The results are shown in Table 3.
Table 3 Different Alkali catalyzer is to SiO 2the impact of aerogel density
Embodiment Alkaline catalysts Density (kg/m 3）
11 Potassium hydroxide 51
12 Sodium hydroxide 67
13 Ammoniacal liquor 76
Embodiment 14～18: different digestion times are to SiO 2the impact of aerogel density
According to the method for embodiment 3, get tetraethoxy 4mL, by V (TEOS): V (H 2o): V (EtOH) is for the mixing solutions of 1:2:5 stirs, and other operate with embodiment 3, and different is to change digestion time, and embodiment 14 is 6h, and embodiment 15 is 12h, and embodiment 16 is 18h, and embodiment 17 is 24h, and embodiment 18 is 36h.The results are shown in Table 4.
The different digestion times of table 4 are to SiO 2the impact of aerogel density
Embodiment Digestion time (h) Density (kg/m 3）
14 6 78
15 12 49
16 18 65
17 24 70
18 36 79
Embodiment 19～23 different solvents time swaps are to SiO 2the impact of aerogel density
According to the method for embodiment 4, get tetraethoxy 4mL, adopt V (TEOS): V (H 2o): the mixing solutions that V (EtOH) is 1:3:7, other operate with embodiment 4, and different is to change the solvent exchange time, and embodiment 19 is 6h, and embodiment 20 is 12h, and embodiment 21 is 18h, and embodiment 22 is 24h, and embodiment 23 is 36h.The results are shown in Table 5.
Table 5 different solvents time swap is to SiO 2the impact of aerogel density
Embodiment The solvent exchange time (h) Density (kg/m 3）
19 6 67
20 12 55
21 18 62
22 24 74
23 36 80
The volume ratio of the different trimethylchlorosilanes of embodiment 24～28 and normal hexane is to SiO 2the impact of aerogel density
According to the method for embodiment 5, get tetraethoxy 4mL, adopt V (TEOS): V (H 2o): the mixing solutions that V (EtOH) is 1:4:9, other operations are with embodiment 5, different is the volume ratio that changes trimethylchlorosilane and normal hexane, embodiment 24 is 1:100, embodiment 25 is 5:100, embodiment 26 is 20:100, and embodiment 27 is 35:100, and embodiment 28 is 50:100.The results are shown in Table 6.
The volume ratio of the different trimethylchlorosilanes of table 6 and normal hexane is to SiO 2the impact of aerogel density
Embodiment V (TMCS): the V(normal hexane) Density (kg/m 3）
24 1：100 79
25 5：100 51
26 20：100 59
27 35：100 64
28 50：100 77
The different drying temperatures of embodiment 29～33 are to SiO 2the impact of aerogel density
According to the method for embodiment 4, get tetraethoxy 4mL, adopt V (TEOS): V (H 2o): the mixing solutions that V (EtOH) is 1:3:7, other operate with embodiment 4, and different is to change drying temperature, and embodiment 29 is 30 ℃, and embodiment 30 is 50 ℃, and embodiment 31 is 100 ℃, and embodiment 32 is 150 ℃, and embodiment 33 is 250 ℃.The results are shown in Table 7.
The different drying temperatures of table 7 are to SiO 2the impact of aerogel density
Embodiment Drying temperature (℃) Density (kg/m 3）
29 30 65
30 50 50
31 100 61
32 150 63
33 250 78
[0055]at present, document and the standby SiO of patent system of open report 2aerogel density is at 55～220kg/m 3between, major part concentrates on 110～220kg/m 3, and SiO prepared by the present invention 2the aerogel density range is 50～80kg/m 3, the SiO prepared under the normal temperature and pressure conditions of generally openly reporting lower than great majority 2the density of aerogel; Document and the patent of open report prepare SiO under the constant pressure and dry condition 2the time of aerogel was at 6～14 days, and the present invention only needs 1～3 day, had significantly shortened SiO 2the preparation cycle of aerogel, and raw material of the present invention is easy to get, technique is simple, and preparation cost is low, is easy to suitability for industrialized production.

Claims (8)

1. prepare the method for low-density silicon dioxide aerogel under a normal pressure, it is characterized in that described method comprises the steps:
By tetraethoxy, water and ethanol are that the ratio of 1:0.5～19:1～29 is mixed by volume, adding sour adjust pH is 3～4, catalytic hydrolysis 30～40 minutes, obtain silicon sol, adding the adjusting PH with base value is 6～6.5 again, catalysis gel 8～10 minutes, obtain wet gel, by wet gel aging 6～36h at room temperature, add normal hexane to carry out solvent exchange 6～36h, gel after displacement is immersed in the mixing solutions of trimethylchlorosilane and normal hexane and carries out hydrophobically modified 12～15 hours, then remove modification liquid with the normal hexane washing, put into again retort furnace and be warming up to 30～250 ℃ of dryings, last cool to room temperature makes aerosil, described acid is mineral acid, monobasic organic acid or binary organic acid, described alkali is mineral alkali, in the mixing solutions of described trimethylchlorosilane and normal hexane, the volume ratio of trimethylchlorosilane and normal hexane is 1～50:100.
2. the method for claim 1, the volume ratio that it is characterized in that described tetraethoxy, water and ethanol is 1:0.5～4:1～9.
3. the method for claim 1, is characterized in that described acid is formic acid, nitric acid, phenylformic acid, hydrochloric acid or acetic acid.
4. the method for claim 1, is characterized in that described alkali is potassium hydroxide, sodium hydroxide or ammoniacal liquor.
5. the method for claim 1, is characterized in that in the mixing solutions of described trimethylchlorosilane and normal hexane, and the volume ratio of trimethylchlorosilane and normal hexane is 5～35:100.
6. the method for claim 1, the temperature that it is characterized in that described drying is 50～150 ℃.
7. the method for claim 1,10～15 times of the volume that the volumetric usage that it is characterized in that the described normal hexane for solvent exchange is tetraethoxy.
8. the method for claim 1,10～15 times of the volume that the volumetric usage that it is characterized in that the mixing solutions of described trimethylchlorosilane and normal hexane is tetraethoxy.
CN2013102727158A 2013-06-29 2013-06-29 Method for preparing low density silica aerogel under normal pressure Pending CN103435055A (en)

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Application publication date: 20131211