CN103213996B - A kind of preparation method of multi-stage porous silicon dioxide base composite aerogel - Google Patents
A kind of preparation method of multi-stage porous silicon dioxide base composite aerogel Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of multi-stage porous silicon dioxide base aerogel composite, relate to field of inorganic materials.Its preparation method is colloidal sol after the mesoporous silica molecular sieve add process in precursor solution after, then adds catalyzer and makes its gel, eventually passes supercritical drying/modification and constant pressure and dry prepares multi-stage porous aerogel composite.The invention has the advantages that: 1) obtained multi-stage porous silicon dioxide base aerogel composite by supercritical drying or atmosphere pressure desiccation.2) by multi-stage porous silicon dioxide base aerogel composite prepared by method provided by the invention, product microtexture is even, and intensity is high, and heat-insulating property is good, and density is low and specific surface area is high.3) with method preparation technology provided by the invention is simple, reaction conditions is gentle, flow process is short, suitability for industrialized production is applicable to.
Description
Technical field
The invention belongs to inorganic thermal insulation material field, be specifically related to a kind of multi-stage porous silicon dioxide base composite aerogel and preparation method thereof.
Background technology
Aerosil refers to the nanoporous silica cross-linked network structure mutually assembling formation with nanometer scale ultrafine particle, containing being greater than the air of 90% and being less than the solid silica skeleton of 10%.The structure of aerosil uniqueness makes it have excellent performance: extremely low density and thermal conductivity, very high specific surface area and porosity.In addition, aerosil also has that low-refraction, Young's modulus are little, numerous excellent characteristic such as low acoustic impedance and high adsorption capacity.Therefore, aerosil has at basic scientific research, building, military project, aerospace and industrial circle and applies comparatively widely.
But the mesh skeleton structure that aerogel is loose causes its mechanical property poor.Therefore, aerogel is restricted in the application in a lot of field.In order to improve its mechanical property, often need to add the mixture of fiber-like, but mixture and the consistency of aerogel own poor, so the region between mixture and aerogel is comparatively sparse, cause overall ununiformity; Meanwhile, fiber add the density not only substantially increasing aerogel, the significantly reduction of its heat-insulating property and thermotolerance may be caused simultaneously.
United States Patent (USP) the 5th, 786, No. 059 discloses a kind of preparation method aerogel particle being evenly sprayed at the polymer formation bi-component fiber material that two kinds are firmly connected together.Its sample hardness prepared is comparatively large, but under external force can be broken, and namely the bonding force of fiber and aerogel is not enough, does not also possess the characteristic of applied at elevated temperature simultaneously.Publication number is that the Chinese patent of CN102807358A provides a kind of Flexible aerogel block and preparation method thereof, its obtained aerogel has good flexibility, but its density, specific surface area pure silicon dioxide aerogel relative to thermal conductivity, there is a certain distance, and do not possess flame-retarding characteristic.Publication number is the preparation method that the Chinese patent of CN102531536A provides a kind of fire-retardant silica aerogel heat insulation composite material.Flame-retardant heat insulating effect is better, but its preparation method is comparatively complicated, and higher to equipment requirements in preparation process.Publication number is the preparation method that the Chinese patent of CN101792299A provides a kind of heat-resisting alumina-silox aerogel thermal-protective composite material, obtained aerogel has that use temperature is high, heat-proof quality good, mechanical strength high, but its preparation process is quite complicated.
In sum, in order to overcome the poor inferior position of mechanical property, other materials composite aerogel is used to be a kind of practicable thinking.But at present the preparation method of composite aerogel can cause uneven, the problem such as preparation process is complicated of aerogel structure, and the advantage such as low density, lower thermal conductivity of silica aerogel may be reduced.Therefore, we have proposed a kind of preparation method of multi-stage porous silicon dioxide base composite aerogel: on the one hand, because mesoporous silica molecular sieve and nanoporous silica matrices are unbodied silicon-dioxide, therefore its consistency is better, makes composite aerogel, relative to density, thermal conductivity pure silicon dioxide aerogel, too large change can not occur; On the other hand, because most si molecular sieves is bar-shaped formation, in aerogel gelation process, not only become nucleating center, certain enhancement can be played to aerogel skeleton simultaneously.
Summary of the invention
The object of the present invention is to provide the preparation method of the multi-stage porous silicon dioxide base composite aerogel that a kind of technique is simple, mild condition, flow process are short, to overcome the deficiency of above-mentioned preparation method, and ensure that the product microtexture obtained is even, intensity is high, heat-insulating property is good, and density is low and specific surface area is high.
Technical scheme of the present invention is: in precursor solution, a) add the mesoporous silica molecular sieve after process, ultrasonicly makes it dispersed; B) colloidal sol is obtained; C) add catalyzer and make its gel, obtain silica-base composite material; D) multi-stage porous aerogel composite is prepared through supercritical drying/modification and constant pressure and dry.Obtained multi-stage porous silicon dioxide composite aerogel density of material is 0.03 ~ 0.60g/cm
3, porosity is 85 ~ 99.5%, and specific surface area is 500 ~ 1000m
2/ g, thermal conductivity is 0.02 ~ 0.05Wm
-1k
-1.
Concrete preparation process is:
1. supercritical drying preparation process, comprises the following steps:
1) by deionized water, dehydrated alcohol, presoma silicon source and 0.1 ~ 1mol/L acid catalyst with volume ratio be 1:0.5 ~ 5:0.5 ~ 2:0.005 ~ 0.1 ratio uniform mixing, after stirring, mesoporous silica molecular sieve powder is added in the ratio of every 50mL mixing solutions 0.005 ~ 0.1g, after stirring, ultrasonic 10 ~ 30min, then left at room temperature 10min ~ 12h;
2) alkaline catalysts of 0.01 ~ 1mol/L of mixing solutions cumulative volume 16% ~ 30% of the ionized water that accounts for, dehydrated alcohol, presoma silicon source and 0.1 ~ 1mol/L acid catalyst is added in the mixing solutions obtained in step 1), in left at room temperature 12 ~ 240h, obtain the gel of homogeneous transparent; Described alkaline catalysts comprises: ammoniacal liquor, Monoethanolamine MEA BASF, the one in diethanolamine, trolamine
3) at room temperature above-mentioned gel is placed in dehydrated alcohol and carries out replacement(metathesis)reaction, replace 3 ~ 10 times, each 12 ~ 48h.
4) the block mixture obtained is placed in airtight high-temperature high-pressure reaction kettle, is warming up to 260 ~ 300 DEG C with the speed of 5 ~ 20 DEG C/min, be incubated after 3 ~ 10 hours, relief pressure in 1 ~ 5 hour, multi-stage porous silicon dioxide composite aerogel material can be obtained.
Further, described presoma silicon source comprises the one in tetraethoxy, methyl silicate; Described mesoporous silica molecular sieve comprises: one or more in SBA-15, MCM-41, MCM-48; Described acid catalyst comprises: the one in hydrochloric acid, oxalic acid, citric acid.
Preferably, described presoma silicon source is tetraethoxy; Described mesoporous silica molecular sieve is SBA-15; Described acid catalyst is hydrochloric acid; Described alkaline catalysts is ammoniacal liquor.
2. constant pressure and dry preparation process, comprises the following steps:
1) to the pre-treatment of mesoporous silica molecular sieve, step is comprised:
1.1) be that the ratio of 10:7 ~ 3:1 mixes with volume ratio by the hydrogen peroxide of the vitriol oil and 30%.
1.2) above-mentioned solution mesoporous silica molecular sieve powder being placed in 60 DEG C ~ 100 DEG C soaks 1 ~ 5h, then centrifugation, uses deionized water and absolute ethanol washing 3 ~ 5 times respectively, centrifugation;
1.3), after the mesoporous silica molecular sieve powder obtained being placed in the dry 6 ~ 12h of 60 DEG C ~ 100 DEG C thermostatic drying chambers, room temperature is cooled to.
2) by deionized water, dehydrated alcohol, presoma silicon source and 0.1 ~ 1mol/L acid catalyst with volume ratio be 1:0.5 ~ 5:0.5 ~ 2:0.005 ~ 0.1 ratio uniform mixing, after stirring, above-mentioned treated mesoporous silica molecular sieve powder is added in the ratio of every 50mL mixing solutions 0.005 ~ 0.1g, after stirring, ultrasonic 10 ~ 30min, then left at room temperature 10min ~ 12h;
3) to step 2) in add the alkaline catalysts of 0.01 ~ 1mol/L of mixing solutions cumulative volume 16% ~ 30% of the ionized water that accounts for, dehydrated alcohol, presoma silicon source and 0.1 ~ 1mol/L acid catalyst in the mixing solutions that obtains, in left at room temperature 12 ~ 240h, obtain the gel of homogeneous transparent;
4) above-mentioned gel is placed in tensio-active agent, at room temperature carries out replacement(metathesis)reaction, replace 3 ~ 10 times, each 12 ~ 48h;
5) gel after displacement being added volume is deionized water, dehydrated alcohol, the surface-modifying agent of mixing solutions cumulative volume 30% ~ 100% of presoma silicon source and 0.1 ~ 1mol/L acid catalyst and modification 24h ~ 72h in tensio-active agent mixing solutions, and wherein surface-modifying agent and tensio-active agent volume are than being 1:5 ~ 15;
6) the above-mentioned gel through modification is placed in tensio-active agent, at room temperature carries out replacement(metathesis)reaction, replace 3 ~ 10 times, each 12 ~ 48h.
7) be uncoveredly placed in the dry 72h ~ 240h of thermostat container that temperature is room temperature, be placed on dry 1 ~ 3h in the baking oven of 200 DEG C.
Further, the mesoporous silica molecular sieve in described step 1) comprises: one or more in SBA-15, MCM-41, MCM-48.
Further, described mesoporous silica molecular sieve is SBA-15.
Further, described presoma silicon source comprises the wherein one in tetraethoxy, methyl silicate; Described acid catalyst comprises: the one in hydrochloric acid, oxalic acid, citric acid; Described alkaline catalysts comprises: ammoniacal liquor, Monoethanolamine MEA BASF, the one in diethanolamine, trolamine; Described tensio-active agent is the one in normal hexane, Skellysolve A, methylacetone, isopropylcarbinol; Described surface-modifying agent is the one in methyl trimethoxy oxygen radical siloxane, Union carbide A-162, dimethylchlorosilane, ethoxytrimethylsilane, hexamethyldisilazane, vinyltriethoxysilane, phenyl triethoxysilane, trimethylchlorosilane.
Preferably, described presoma silicon source is tetraethoxy; Described acid catalyst is hydrochloric acid; Described alkaline catalysts is ammoniacal liquor; Described tensio-active agent is normal hexane; Described surface-modifying agent is trimethylchlorosilane.
The invention has the advantages that: 1) obtained multi-stage porous silicon dioxide base aerogel composite by supercritical drying or atmosphere pressure desiccation.2) by multi-stage porous silicon dioxide base aerogel composite prepared by method provided by the invention, product microtexture is even, and intensity is high, and heat-insulating property is good, and density is low and specific surface area is high.3) with method preparation technology provided by the invention is simple, reaction conditions is gentle, flow process is short, suitability for industrialized production is applicable to.
Specific embodiments
Below in conjunction with specific embodiments, the present invention is further elaborated.
Case study on implementation 1
A) by the hydrochloric acid of deionized water, dehydrated alcohol, tetraethoxy and 0.25mol/L with volume ratio be 1:1.5:1.5:0.05 ratio uniform mixing, cumulative volume is 50mL, after stirring, add 0.01gSBA-15 powder, after stirring, ultrasonic 10min in ultrasonic wave, and be placed on standing 2h in room temperature.
B) add the ammonia soln of 10mL0.5mol/L, in left at room temperature 48h, obtain the gel of homogeneous transparent;
C) at room temperature above-mentioned gel is placed in dehydrated alcohol and carries out replacement(metathesis)reaction, replace 5 times, each 24h;
D) the block mixture obtained is placed in airtight high-temperature high-pressure reaction kettle, is warming up to 260 DEG C with the speed of 5 DEG C/min, be incubated after 5 hours, relief pressure in 2 hours, multi-stage porous silicon dioxide composite aerogel material can be obtained.
Case study on implementation 2
A) by the oxalic acid of deionized water, dehydrated alcohol, tetraethoxy and 0.5mol/L with volume ratio be 1:1.5:1.5:0.1 ratio uniform mixing, cumulative volume is 50mL, after stirring, add 0.01gSBA-15 powder, after stirring, ultrasonic 10min in ultrasonic wave, and be placed on standing 2h in room temperature.
B) add the ammonia soln of 10mL0.5mol/L, in left at room temperature 48h, obtain the gel of homogeneous transparent;
C) at room temperature above-mentioned gel is placed in dehydrated alcohol and carries out replacement(metathesis)reaction, replace 5 times, each 24h;
D) the block mixture obtained is placed in airtight high-temperature high-pressure reaction kettle, is warming up to 260 DEG C with the speed of 5 DEG C/min, be incubated after 5 hours, relief pressure in 2 hours, multi-stage porous silicon dioxide composite aerogel material can be obtained.
Case study on implementation 3
A) be that the ratio of 7:3 mixes with volume ratio by the hydrogen peroxide of the vitriol oil and 30%.
B) above-mentioned solution MCM-41 powder being placed in 100 DEG C soaks 3h, then to obtaining SiO 2 molecular sieve powder, (general centrifugal speed is 10000 turns/min in centrifugation, centrifugal about 5 ~ 10min), use deionized water and absolute ethanol washing 3 times respectively, centrifugation is to obtaining SiO 2 molecular sieve powder.
C), after the mesoporous silica molecular sieve powder obtained being placed in 80 DEG C of dry 8h of thermostatic drying chamber, room temperature is cooled to.
D) by the hydrochloric acid of deionized water, dehydrated alcohol, tetraethoxy and 0.25mol/L with volume ratio be 1:1.5:1.5:0.05 ratio uniform mixing, cumulative volume is 50mL, after stirring, add the above-mentioned treated MCM-41 powder of 0.01g, after stirring, ultrasonic 10min in ultrasonic wave, and be placed in normal temperature and keep 2h.
E) add the ammonia soln of 10mL0.5mol/L, in left at room temperature 48h, obtain the gel of homogeneous transparent;
F) above-mentioned gel is placed in normal hexane, at room temperature carries out replacement(metathesis)reaction, replace 5 times, each 12h;
G) hexane solution (wherein the volume ratio of trimethylchlorosilane is 10%) the modification 24h of 30mL trimethylchlorosilane is added;
H) the above-mentioned gel through modification is placed in normal hexane, at room temperature carries out replacement(metathesis)reaction, replace 5 times, each 12h;
I) be uncoveredly placed in the dry 72h of thermostat container that temperature is room temperature, be placed on dry 2h in the baking oven of 200 DEG C.
Above case study on implementation is only used to the principal character and the ultimate principle that show and describe patent of the present invention, and the present invention is not by the restriction of above-mentioned true case, and application claims protection domain is defined by claims and equivalent thereof.
Claims (9)
1. a preparation method for multi-stage porous silicon dioxide base composite aerogel, is characterized in that: comprise the following steps:
1) by deionized water, dehydrated alcohol, presoma silicon source and 0.1 ~ 1mol/L acid catalyst with volume ratio be 1:0.5 ~ 5:0.5 ~ 2:0.005 ~ 0.1 ratio uniform mixing, after stirring, mesoporous silica molecular sieve powder is added in the ratio of every 50mL mixing solutions 0.005 ~ 0.1g, after stirring, ultrasonic 10 ~ 30min, then left at room temperature 10min ~ 12h;
2) alkaline catalysts of 0.01 ~ 1mol/L of mixing solutions cumulative volume 16% ~ 30% of the ionized water that accounts for, dehydrated alcohol, presoma silicon source and 0.1 ~ 1mol/L acid catalyst is added in the mixing solutions obtained in step 1), in left at room temperature 12 ~ 240h, obtain the gel of homogeneous transparent; Described alkaline catalysts comprises: ammoniacal liquor, Monoethanolamine MEA BASF, the one in diethanolamine, trolamine;
3) at room temperature above-mentioned gel is placed in dehydrated alcohol and carries out replacement(metathesis)reaction, replace 3 ~ 10 times, each 12 ~ 48h;
4) the block mixture obtained is placed in airtight high-temperature high-pressure reaction kettle, is warming up to 260 ~ 300 DEG C with the speed of 5 ~ 20 DEG C/min, be incubated after 3 ~ 10 hours, relief pressure in 1 ~ 5 hour, multi-stage porous silicon dioxide composite aerogel material can be obtained.
2. according to the preparation method of multi-stage porous silicon dioxide base composite aerogel according to claim 1, it is characterized in that: described presoma silicon source comprises the one in tetraethoxy, methyl silicate; Described mesoporous silica molecular sieve comprises: one or more in SBA-15, MCM-41, MCM-48; Described acid catalyst comprises: the one in hydrochloric acid, oxalic acid, citric acid.
3. according to the preparation method of multi-stage porous silicon dioxide base composite aerogel according to claim 1 and 2, it is characterized in that: described presoma silicon source is tetraethoxy; Described mesoporous silica molecular sieve is SBA-15; Described acid catalyst is hydrochloric acid; Described alkaline catalysts is ammoniacal liquor.
4. a preparation method for multi-stage porous silicon dioxide base composite aerogel, is characterized in that: comprise the following steps:
1) to the pre-treatment of mesoporous silica molecular sieve, step is comprised:
1.1) be that the ratio of 10:7 ~ 3:1 mixes with volume ratio by the hydrogen peroxide of the vitriol oil and 30%;
1.2) above-mentioned solution mesoporous silica molecular sieve powder being placed in 60 DEG C ~ 100 DEG C soaks 1 ~ 5h, then centrifugation, uses deionized water and absolute ethanol washing 3 ~ 5 times respectively, centrifugation;
1.3), after the mesoporous silica molecular sieve powder obtained being placed in the dry 6 ~ 12h of 60 DEG C ~ 100 DEG C thermostatic drying chambers, room temperature is cooled to;
2) by deionized water, dehydrated alcohol, presoma silicon source and 0.1 ~ 1mol/L acid catalyst with volume ratio be 1:0.5 ~ 5:0.5 ~ 2:0.005 ~ 0.1 ratio uniform mixing, after stirring, above-mentioned treated mesoporous silica molecular sieve powder is added in the ratio of every 50mL mixing solutions 0.005 ~ 0.1g, after stirring, ultrasonic 10 ~ 30min, then left at room temperature 10min ~ 12h;
3) to step 2) in add the alkaline catalysts of 0.01 ~ 1mol/L of mixing solutions cumulative volume 16% ~ 30% of the ionized water that accounts for, dehydrated alcohol, presoma silicon source and 0.1 ~ 1mol/L acid catalyst in the mixing solutions that obtains, in left at room temperature 12 ~ 240h, obtain the gel of homogeneous transparent;
4) above-mentioned gel is placed in tensio-active agent, at room temperature carries out replacement(metathesis)reaction, replace 3 ~ 10 times, each 12 ~ 48h; Described tensio-active agent is the one in normal hexane, Skellysolve A, methylacetone, isopropylcarbinol;
5) gel after displacement being added volume is deionized water, dehydrated alcohol, the surface-modifying agent of mixing solutions cumulative volume 30% ~ 100% of presoma silicon source and 0.1 ~ 1mol/L acid catalyst and modification 24h ~ 72h in tensio-active agent mixing solutions, and wherein surface-modifying agent and tensio-active agent volume are than being 1:5 ~ 15; Described surface-modifying agent is the one in methyl trimethoxy oxygen radical siloxane, Union carbide A-162, dimethylchlorosilane, ethoxytrimethylsilane, hexamethyldisilazane, vinyltriethoxysilane, phenyl triethoxysilane, trimethylchlorosilane;
6) the above-mentioned gel through modification is placed in tensio-active agent, at room temperature carries out replacement(metathesis)reaction, replace 3 ~ 10 times, each 12 ~ 48h;
7) be uncoveredly placed in the dry 72h ~ 240h of thermostat container that temperature is room temperature, be placed on dry 1 ~ 3h in the baking oven of 200 DEG C.
5. the preparation method of multi-stage porous silicon dioxide base composite aerogel according to claim 4, is characterized in that: the mesoporous silica molecular sieve in described step 1) comprises: one or more in SBA-15, MCM-41, MCM-48.
6. the preparation method of multi-stage porous silicon dioxide base composite aerogel according to claim 5, is characterized in that: described mesoporous silica molecular sieve is SBA-15.
7. the preparation method of multi-stage porous silicon dioxide base composite aerogel according to claim 4, is characterized in that: described presoma silicon source comprises the wherein one in tetraethoxy, methyl silicate; Described acid catalyst comprises: the one in hydrochloric acid, oxalic acid, citric acid; Described alkaline catalysts comprises: ammoniacal liquor, Monoethanolamine MEA BASF, the one in diethanolamine, trolamine.
8. the preparation method of the multi-stage porous silicon dioxide base composite aerogel according to claim 4 or 7, is characterized in that: described presoma silicon source is tetraethoxy; Described acid catalyst is hydrochloric acid; Described alkaline catalysts is ammoniacal liquor; Described tensio-active agent is normal hexane; Described surface-modifying agent is trimethylchlorosilane.
9. the preparation method of the multi-stage porous silicon dioxide base composite aerogel according to claim 1 or 4, is characterized in that: described obtained multi-stage porous silicon dioxide composite aerogel density of material is 0.03 ~ 0.60g/cm
3, porosity is 85 ~ 99.5%, and specific surface area is 500 ~ 1000m
2/ g, thermal conductivity is 0.02 ~ 0.05Wm
-1k
-1.
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| JP2005247661A (en) * | 2004-03-05 | 2005-09-15 | Matsushita Electric Works Ltd | Silica aerogel, method for manufacturing silica aerogel, and apparatus for detecting elementary particle |
| CN101628804A (en) * | 2008-07-18 | 2010-01-20 | 山东鲁阳股份有限公司 | Aerogel heat insulation composite material and preparation method thereof |
| CN101973752B (en) * | 2010-10-21 | 2013-01-23 | 厦门大学 | Glass fiber reinforced silicon dioxide aerogel composite material and preparation method thereof |
| CN103011745A (en) * | 2012-11-27 | 2013-04-03 | 天津大学 | Silicon-dioxide aerogel heat insulation composite material and preparation method thereof |
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