CN106745001A - A kind of A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method - Google Patents
A kind of A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method Download PDFInfo
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- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
- C01B33/166—Preparation of silica xerogels by acidification of silicate in the presence of an inert organic phase
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Abstract
The invention discloses a kind of A grades non-combustible hydrophobic silica aerogel powder atmospheric preparation method, including：Waterglass and water are uniformly mixing to obtain mixed liquor A；Under stirring, by mixed liquor A add acid solution in, pH value determination, the 10min of collosol and gel 2 obtains wet gel after pH reaches predetermined value, wet gel is carried out at normal temperatures aging；Wet gel after will be aging is crushed and obtains gel particle；To adding non-polar solven, alcohols and silane coupler to swap and be modified as modifier solution in gel particle, modified wet gel particle is obtained after removing modifier solution, modified wet gel particle drying is obtained into gel powder；Gel powder is put into Muffle furnace and is heat-treated.A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method proposed by the present invention, low cost, efficiency high, cycle is short, favorable repeatability, the A for obtaining grades of non-combustible hydrophobic silica aerogel powder excellent fireproof performance, hydrophobicity is good.
Description
Technical field
The present invention relates to aerosil preparing technical field, more particularly to a kind of A grades of non-combustible hydrophobic silica
Aerogel powder atmospheric preparation method.
Background technology
The important technology that nanometer technology has developed since being the eighties in last century, nanometer science and technology is considered as 21
Century three one of big science and technology, its scientific value and application prospect are gradually recognized by people.Nanometer technology is in numerous areas
Wide space is presented using for heat-barrier material.SiO2Aerogel material its unique nano-porous structure so that
Pore diameter is less than gas molecule mean free path, so that the convection heat transfer' heat-transfer by convection of gas molecule is limited, while the superelevation porosity makes again
The solid phase heat transfer for obtaining material is restricted, therefore SiO2Aeroge is a kind of novel nano heat-barrier material, and it is led under normal temperature and pressure
Hot coefficient is less than air.With excellent thermal insulation performance, while SiO2Amorphous solid with very high porosities, chemical stability
It is good, it is harmless.In civil area, aerogel heat-insulating material as a kind of New Building Materials, with thermally-stabilised well
Property, resistance to sudden heating and heat-insulation warm keeping.In field of aerospace, the aerogel heat-insulating composite material with low-density can be used
Lighter quality, smaller volume reach the effect of heat insulation equivalent with traditional insulation materials.In energy-conserving and environment-protective, new energy field etc.
Play the role of irreplaceable.
At present, SiO2The preparation method of aeroge mainly includes supercritical drying and constant pressure and dry two ways.It is overcritical
SiO prepared by method2Aeroge performance is more excellent, but the power consumption of equipment complex and expensive, drying process is high, dangerous big；Normal pressure is done
Dry preparation SiO2Without large number quipments, workable, safety and environmental protection is SiO to aeroge2The large-scale industry metaplasia of aeroge
Produce there is provided possible.But the normal pressure preparation technology of report is cumbersome at present, easily there is modified incomplete, the SiO for preparing2Gas
Gel powder is poor quality, and time-consuming to produce manufacturing cycle, and a large amount of hydrophobic modifiers and displacement solvent are expended in production,
And solvent recovery separates difficulty, the skill cycle is long, prepares environment and does not fix, and causes SiO2The repeatability of aeroge performance is poor, increases
Add the cost of product, and combustibility can not reach A grades of fire resistance, so as to the industrialization for limiting aeroge is extensive
Prepare and extensive use.
Secondly, current SiO2The preparation of aerogel powder is usually to clay into power again or use using preparing aerogel block body
Spray-on process or emulsion method.The SiO that spray-on process is prepared2Then easily drop produces adhesion to aerogel powder during spraying
Reunite, so as to powder of the particle diameter more than 1mm occur；The SiO that emulsion method is prepared2Aeroge then due to emulsion droplet size not
Homogeneous, the aerogel powder particle size distribution range for preparing is wide.
Chinese patent CN102557052A refer to a kind of method of quick preparation low-density silicon oxide aerogel, provide
SiO2Hydrogel；To the SiO2Hydrogel carries out microwave irradiation so that it reaches complete gelation；Successively with polar solvent and non-
Polar solvent carries out solvent displacement to the hydrogel of resulting complete gelation；Obtain low-density silicon oxide aerogel.But institute
Prepare aeroge and do not reach A grades of flame retardant effect.
Chinese patent CN104891509A refer to a kind of fast preparation method of A grades of non-combustible silica aerogel, the party
Method is combined using alkaline sol with inorganic material, is placed in CO2It is dried in overcritical device, is finally sprayed onto silane modifier
Silicon oxide surface is dried, heating is obtained.The aeroge glass composite blanket reach A grades it is non-combustible, with good hydrophobic performance, but need
Supercritical drying is wanted, cost is larger, it is impossible to meet the demand of industrialized production.
Chinese patent CN102602943A refer to the side that one-step method quickly prepares high-performance nano silicon dioxide aerogel
Method, organosilicon is mixed in container in mass ratio with solvent, after mixing with catalyst quality ratio according to water, the catalyst is molten
Liquid is slowly added into the foregoing mixed solution in stirring, and container closure is waited into age gelation, is drying to obtain silica gas
Gel.Made aeroge does not reach A grades of fire resistance.
A kind of SiO is mentioned in Chinese patent CN102079949A2Aeroge constant pressure and dry technique, with trim,ethylchlorosilane
(TMCS) and n-hexane mixed liquor as modifying agent, 3-5 subsurfaces are carried out to the gel after aging and are modified, each modification time
It it is 24-48 hours, modifying process is cumbersome in the patent, only modifying process is accomplished by more than 3 days, is unfavorable for SiO2The product of aeroge
Industry metaplasia is produced.
Chinese patent CN102951650A refer to a kind of quick preparation SiO2The constant pressure and dry method of aeroge, by with
Low surface tension solvent replaces part alcoholic solvent, according to a certain ratio by silicon alkoxide, alcoholic solvent, acidic catalyst, base catalyst
And low surface tension solvent is configured to colloidal sol, after forming the alcogel containing low surface tension solvent, after aging, surface modification
Constant pressure and dry directly is carried out, SiO is prepared in 30 hours2Aeroge.
Chinese patent CN102897778A refer to the preparation method of nano silica aerogel powder：Prepare first molten
Glue, then carries out in-situ modified to colloidal sol, is finally dried modified colloidal sol, obtains nanometer titanium dioxide silica aerogel powder
Body.
Chinese patent CN101691227 refer to the preparation method of silica aerogel material, using positive silicic acid tetrem
Ester is silicon source, and MTMS or MTES are co-precursor modifying agent, and absolute ethyl alcohol is solvent, salt
Acid and ammoniacal liquor are catalyst.SiO is obtained using the catalysis of sol-gel soda acid two-step method2Wet gel, is carried out old under certain condition
After change treatment, to wet gel sample modification again, and the final atmospheric low-temperature in air atmosphere is dried to obtain SiO2Airsetting
Glue.
The content of the invention
Based on the technical problem that background technology is present, the present invention proposes a kind of A grades of non-combustible hydrophobic silica aerogel
Powder atmospheric preparation method, its low cost, efficiency high, cycle is short, favorable repeatability, the A for obtaining grades of non-combustible hydrophobic silica
Aerogel powder excellent fireproof performance, hydrophobicity is good.
A kind of A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method proposed by the present invention, including following step
Suddenly：
S1, waterglass and water are uniformly mixing to obtain mixed liquor A；
S2, under stirring, during mixed liquor A added into acid solution, and pH value determination stops after pH reaches predetermined value
Only add, wet gel is obtained after collosol and gel 2-10min, wet gel is carried out at normal temperatures aging；
S3, will be aging after wet gel broken obtain gel particle；To in gel particle add non-polar solven, alcohols and
Silane coupler is swapped and is modified as modifier solution, and modified wet gel particle is obtained after removing modifier solution, will
Modified wet gel particle is placed in air dry oven and is dried to obtain gel powder；
S4, gel powder is put into Muffle furnace it is thermally treated resulting in described A grades non-combustible hydrophobic silica aerogel powder.
Preferably, in S1, the modulus of the waterglass is 2.5-3.55, and waterglass and the volume ratio of water are 1：0.5-
1：4.
Preferably, in S2, mixed liquor A is 3-6 with the volume ratio of acid solution：1-3；The acid solution be hydrochloric acid,
One kind in sulfuric acid, oxalic acid, acetic acid.
Preferably, in S2, mixed liquor A is 5 with the volume ratio of acid solution：2.
Preferably, in S2, mixing speed is 200-500r/min；The predetermined value is 4.5-5；Ageing time is 3-
4h。
Preferably, in S3, the non-polar solven is n-hexane, normal heptane, hexamethylene, pentane, petroleum ether, gasoline
In one or more of mixture；The alcohols is the mixture of one or more in ethanol, methyl alcohol, isopropanol.
Preferably, in S3, silane coupler be trim,ethylchlorosilane, HMDS, HMDO,
One kind in APTES.
Preferably, in S3, the gel particle, non-polar solven, alcohols, the volume ratio of silane coupler are 1：2-3：
1-3：2-3.
Preferably, the modifier solution and the volume ratio of gel particle are 6-8：1.
Preferably, in S3, swapped under 50-60 DEG C of water bath condition and modified 3-4h.
Preferably, in S3, drying temperature is 80-120 DEG C.
Preferably, in S4, the temperature of Muffle furnace is 320-380 DEG C, and heat treatment time is 6-7h.
Preferably, in S4, the temperature of Muffle furnace is 350 DEG C, and heat treatment time is 6.5h.
A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method of the present invention, it is any fire-retardant without adding
Agent, i.e., can reach A grades of fire resistance, be provided simultaneously with hydrophobic performance.The equipment for overcoming conventional supercritical fluid drying process is complicated,
Production cost is high, the low shortcoming of efficiency, and it is long also to solve traditional existing constant pressure and dry process cycle, replaces solvent use cost
The problems such as height, poor repeatability.Specifically, the present invention selects industrial waterglass as silicon source, in dispersed phase, in catalyst action
The lower gel particle for forming size uniform, it is modified to it using a step exchange of solvent and surface modifying method, eventually form normal pressure
Drying directly obtains silicon dioxide aerogel powder, can farthest retain the excellent heat-proof quality of aeroge, and have
Hydrophobicity, while greatly reducing the time that colloidal sol is exchanged, surface is modified, is obtained silicon dioxide aerogel powder size uniformity,
Mass energy is saved relative to supercritical drying.
Brief description of the drawings
Fig. 1 is the SEM figures of A grades of non-combustible hydrophobic silica aerogel powder prepared by the embodiment of the present invention 6.
Specific embodiment
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method proposed by the present invention, including following step
Suddenly：
S1, waterglass and water are uniformly mixing to obtain mixed liquor A；
S2, under stirring, during mixed liquor A added into acid solution, and pH value determination stops after pH reaches predetermined value
Only add, wet gel is obtained after collosol and gel 10min, wet gel is carried out at normal temperatures aging；
S3, will be aging after wet gel broken obtain gel particle；To in gel particle add non-polar solven, alcohols and
Silane coupler is swapped and is modified as modifier solution, and modified wet gel particle is obtained after removing modifier solution, will
Modified wet gel particle is placed in air dry oven and is dried to obtain gel powder；
S4, gel powder is put into Muffle furnace it is thermally treated resulting in described A grades non-combustible hydrophobic silica aerogel powder.
Embodiment 2
A kind of A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method proposed by the present invention, including following step
Suddenly：
S1, waterglass and water are uniformly mixing to obtain mixed liquor A；
S2, under stirring, during mixed liquor A added into acid solution, and pH value determination stops after pH reaches predetermined value
Only add, wet gel is obtained after collosol and gel 2min, wet gel is carried out at normal temperatures aging；
S3, will be aging after wet gel broken obtain gel particle；To in gel particle add non-polar solven, alcohols and
Silane coupler is swapped and is modified as modifier solution, and modified wet gel particle is obtained after removing modifier solution, will
Modified wet gel particle is placed in air dry oven and is dried to obtain gel powder；
S4, gel powder is put into Muffle furnace it is thermally treated resulting in described A grades non-combustible hydrophobic silica aerogel powder.
Embodiment 3
A kind of A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method proposed by the present invention, including following step
Suddenly：
S1, waterglass and water are uniformly mixing to obtain mixed liquor A；Wherein, the modulus of the waterglass is 2.5, and water glass
Glass is 1 with the volume ratio of water：0.5；
S2, under stirring, during mixed liquor A added into acid solution, and pH value determination stops after pH reaches predetermined value
Only add, wet gel is obtained after collosol and gel 3min, wet gel is carried out at normal temperatures aging；Wherein, mixed liquor A is molten with acidity
The volume ratio of liquid is 6：1；The acid solution is sulfuric acid；Mixing speed is 500r/min；The predetermined value is 4.5；When aging
Between be 4h；
S3, will be aging after wet gel broken obtain gel particle；To in gel particle add non-polar solven, alcohols and
Silane coupler is swapped and is modified as modifier solution, and modified wet gel particle is obtained after removing modifier solution, will
Modified wet gel particle is placed in air dry oven and is dried to obtain gel powder；Wherein, the non-polar solven is hexamethylene, just
Pentane, petroleum ether are by volume 3：4：1 mixture；The alcohols is isopropanol；Silane coupler is trim,ethylchlorosilane；
The gel particle, non-polar solven, alcohols, the volume ratio of silane coupler are 1：2：3：2；Exchanging and modified process
In, swapped under 50 DEG C of water bath condition and modified 4h；Drying temperature is 80 DEG C；
S4, gel powder is put into Muffle furnace it is thermally treated resulting in described A grades non-combustible hydrophobic silica aerogel powder,
Wherein, the temperature of Muffle furnace is 320 DEG C, and heat treatment time is 7h.
Embodiment 4
A kind of A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method proposed by the present invention, including following step
Suddenly：
S1, waterglass and water are uniformly mixing to obtain mixed liquor A；Wherein, the modulus of the waterglass is 3.55, and water glass
Glass is 1 with the volume ratio of water：4；
S2, under stirring, during mixed liquor A added into acid solution, and pH value determination stops after pH reaches predetermined value
Only add, wet gel is obtained after collosol and gel 8min, wet gel is carried out at normal temperatures aging；Wherein, mixed liquor A is molten with acidity
The volume ratio of liquid is 3：3；The acid solution is hydrochloric acid；Mixing speed is 200r/min；The predetermined value is 5；Ageing time
It is 3h；
S3, will be aging after wet gel broken obtain gel particle；To in gel particle add non-polar solven, alcohols and
Silane coupler is swapped and is modified as modifier solution, and modified wet gel particle is obtained after removing modifier solution, will
Modified wet gel particle is placed in air dry oven and is dried to obtain gel powder；Wherein, the non-polar solven is normal heptane；Institute
It is by volume 3 for ethanol, methyl alcohol, isopropanol to state alcohols：5：2 mixture；Silane coupler is HMDS；Institute
It is 1 to state gel particle, non-polar solven, alcohols, the volume ratio of silane coupler：3：1：3；Exchange with it is modified during,
Swapped under 60 DEG C of water bath condition and modified 3h；Drying temperature is 120 DEG C；
S4, gel powder is put into Muffle furnace it is thermally treated resulting in described A grades non-combustible hydrophobic silica aerogel powder,
Wherein, the temperature of Muffle furnace is 380 DEG C, and heat treatment time is 6h.
Embodiment 5
A kind of A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method proposed by the present invention, including following step
Suddenly：
S1, by modulus be 3 waterglass and water by 1：2 volume ratio is uniformly mixing to obtain mixed liquor A；
S2, under stirring, during mixed liquor A added into acid solution, and pH value determination stops after pH reaches predetermined value
Only add, wet gel is obtained after collosol and gel 5min, wet gel is carried out at normal temperatures aging；Wherein, the acid solution is
Oxalic acid；Mixed liquor A is 5 with the volume ratio of acid solution：2；Mixing speed is 300r/min；The predetermined value is 4.8；When aging
Between be 3.5h；
S3, will be aging after wet gel broken obtain gel particle；To in gel particle add non-polar solven, alcohols and
Silane coupler is swapped and is modified as modifier solution, and modified wet gel particle is obtained after removing modifier solution, will
Modified wet gel particle is placed in air dry oven and is dried to obtain gel powder；Wherein, the non-polar solven is pentane；Institute
Alcohols is stated for ethanol；Silane coupler is APTES；The body of the modifier solution and gel particle
Product is than being 7：1；Swapped under 55 DEG C of water bath condition and modified 3.5h；Drying temperature is 110 DEG C；
S4, gel powder is put into Muffle furnace it is thermally treated resulting in described A grades non-combustible hydrophobic silica aerogel powder,
Wherein, the temperature of Muffle furnace is 350 DEG C, and heat treatment time is 6.5h.
Embodiment 6
A kind of A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method proposed by the present invention, including following step
Suddenly：
S1, by modulus it is waterglass that 3.55, mass fraction is 32.16% and deionized water is by volume 1：4 stirrings
Uniformly obtain mixed liquor A；
S2, under stirring, during 90ml mixed liquor As are added into 18ml concentration for the hydrochloric acid of 5mol/L, stir and measure
PH value, when pH reaches 5, wet gel is obtained after collosol and gel 5min, and wet gel is carried out into aging 4h at normal temperatures；
S3, will be aging after wet gel broken obtain gel particle；To addition 300ml n-hexanes, 300ml in gel particle
Absolute methanol and 220ml trim,ethylchlorosilanes stir 4h and swap and be modified as modifier solution, under 60 DEG C of heating water baths,
Modified wet gel particle is obtained after removing modifier solution, modified wet gel particle is placed in 120 DEG C of air dry oven and is done
It is dry to obtain gel powder；
S4, gel powder is put into Muffle furnace, 350 DEG C of heat treatment 7h obtain described A grades non-combustible hydrophobic silica gas
Gel powder.
Performance test is carried out to A grades manufactured in the present embodiment non-combustible hydrophobic silica aerogel powder, its combustibility A
Non-ignitable, the porosity 91.47% of level, density 0.096g/cm3, thermal conductivity factor 0.0216W/mK, 109.42 ° of hydrophobic angle.
As shown in figure 1, Fig. 1 is the A grades manufactured in the present embodiment SEM figure of non-combustible hydrophobic silica aerogel powder, ginseng
According to A grades of non-combustible hydrophobic silica aerogel powder size uniformity prepared by Fig. 1, the present invention.
Embodiment 7
A kind of A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method proposed by the present invention, including following step
Suddenly：
S1, by modulus it is waterglass that 3.55, mass fraction is 32.16% and deionized water is by volume 2：1 stirring
Uniformly obtain mixed liquor A；
S2, under stirring, during 15ml mixed liquor As are added into 3ml concentration for the hydrochloric acid of 5mol/L, stir and measure pH
Value, when pH reaches 5, wet gel is obtained after collosol and gel 5min, and wet gel is carried out into aging 4h at normal temperatures；
S3, will be aging after wet gel broken obtain gel particle；To added in gel particle 50ml n-hexanes, 50ml without
Water methanol and 36ml trim,ethylchlorosilanes stir 3h and swap and be modified as modifier solution, under 60 DEG C of heating water baths, remove
Modified wet gel particle is obtained after removing modifier solution, modified wet gel particle is placed in 120 DEG C of air dry oven and is dried
Obtain gel powder；
S4, gel powder is put into Muffle furnace, 350 DEG C of heat treatment 6h obtain described A grades non-combustible hydrophobic silica gas
Gel powder.
Performance test is carried out to A grades of the present invention non-combustible hydrophobic silica aerogel powder, A grades of its combustibility is not
Combustion, porosity 90.61%, density 0.082g/cm3, in hydrophobicity, thermal conductivity factor 0.0216W/mK, 108.23 ° of hydrophobic angle.
Embodiment 8
A kind of A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method proposed by the present invention, including following step
Suddenly：
S1, by modulus it is waterglass that 3.55, mass fraction is 32.16% and deionized water is by volume 1：3 stirrings
Uniformly obtain mixed liquor A；
S2, under stirring, during 30ml mixed liquor As are added into 6ml concentration for the hydrochloric acid of 5mol/L, stir and measure pH
Value, when pH reaches 5, wet gel is obtained after collosol and gel 5min, and wet gel is carried out into aging 4h at normal temperatures；
S3, will be aging after wet gel broken obtain gel particle；To addition 100ml n-hexanes, 100ml in gel particle
Absolute methanol and 80ml trim,ethylchlorosilanes stir 3.5h and swap and change as modifier solution, under 55 DEG C of heating water baths
Property, modified wet gel particle is obtained after removing modifier solution, modified wet gel particle is placed in 120 DEG C of air dry oven
It is dried to obtain gel powder；
S4, gel powder is put into Muffle furnace, 350 DEG C of heat treatment 6.5h obtain the A grades of non-combustible hydrophobic silica
Aerogel powder.
Performance test is carried out to A grades of the present invention non-combustible hydrophobic silica aerogel powder, A grades of its combustibility is not
Combustion, porosity 91.78%, density 0.091g/cm3, in hydrophobicity, thermal conductivity factor 0.0212W/mK, 111.45 ° of hydrophobic angle.
Embodiment 9
A kind of A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method proposed by the present invention, including following step
Suddenly：
S1, by modulus it is waterglass that 3.55, mass fraction is 32.16% and deionized water is by volume 1：3 stirrings
Uniformly obtain mixed liquor A；
S2, under stirring, during 60ml mixed liquor As are added into 12ml concentration for the hydrochloric acid of 5mol/L, stir and measure
PH value, when pH reaches 5, wet gel is obtained after collosol and gel 5min, and wet gel is carried out into aging 4h at normal temperatures；
S3, will be aging after wet gel broken obtain gel particle；To addition 200ml n-hexanes, 200ml in gel particle
Absolute methanol and 150ml trim,ethylchlorosilanes stir 3h and swap and be modified as modifier solution, under 60 DEG C of heating water baths,
Modified wet gel particle is obtained after removing modifier solution, modified wet gel particle is placed in 120 DEG C of air dry oven and is done
It is dry to obtain gel powder；
S4, gel powder is put into Muffle furnace, 350 DEG C of heat treatment 6.3h obtain the A grades of non-combustible hydrophobic silica
Aerogel powder.
Performance test is carried out to A grades of the present invention non-combustible hydrophobic silica aerogel powder, A grades of its combustibility is not
Combustion, porosity 91.52%, density 0.095g/cm3, thermal conductivity factor 0.0212W/mK, hydrophobic angle 107.78.
The above, the only present invention preferably specific embodiment, but protection scope of the present invention is not limited thereto,
Any one skilled in the art the invention discloses technical scope in, technology according to the present invention scheme and its
Inventive concept is subject to equivalent or change, should all be included within the scope of the present invention.
Claims (10)
1. a kind of A grades non-combustible hydrophobic silica aerogel powder atmospheric preparation method, it is characterised in that comprise the following steps：
S1, waterglass and water are uniformly mixing to obtain mixed liquor A；
S2, under stirring, during mixed liquor A added into acid solution, and pH value determination, stop after pH reaches predetermined value plus
Enter, wet gel is obtained after collosol and gel 2-10min, wet gel is carried out at normal temperatures aging；
S3, will be aging after wet gel broken obtain gel particle；To addition non-polar solven, alcohols and silane in gel particle
Coupling agent is swapped and is modified as modifier solution, and modified wet gel particle is obtained after removing modifier solution, will be modified
Wet gel particle is placed in air dry oven and is dried to obtain gel powder；
S4, gel powder is put into Muffle furnace it is thermally treated resulting in described A grades non-combustible hydrophobic silica aerogel powder.
2. A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method according to claim 1, it is characterised in that
In S1, the modulus of the waterglass is 2.5-3.55, and waterglass and the volume ratio of water are 1：0.5-1：4.
3. A grades according to claim 1 or claim 2 non-combustible hydrophobic silica aerogel powder atmospheric preparation method, its feature exists
In in S2, mixed liquor A is 3-6 with the volume ratio of acid solution：1-3；The acid solution is hydrochloric acid, sulfuric acid, oxalic acid, vinegar
One kind in acid；Preferably, in S2, mixed liquor A is 5 with the volume ratio of acid solution：2.
4. the A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method according to any one of claim 1-3, its
It is characterised by, in S2, mixing speed is 200-500r/min；The predetermined value is 4.5-5；Ageing time is 3-4h.
5. the A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method according to any one of claim 1-4, its
It is characterised by, in S3, the non-polar solven is in n-hexane, normal heptane, hexamethylene, pentane, petroleum ether, gasoline
Plant or various mixtures；The alcohols is the mixture of one or more in ethanol, methyl alcohol, isopropanol.
6. the A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method according to any one of claim 1-5, its
It is characterised by, in S3, silane coupler is trim,ethylchlorosilane, HMDS, HMDO, 3- amino
One kind in propyl-triethoxysilicane.
7. the A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method according to any one of claim 1-6, its
It is characterised by, in S3, the gel particle, non-polar solven, alcohols, the volume ratio of silane coupler are 1：2-3：1-3：2-
3；Preferably, the modifier solution and the volume ratio of gel particle are 6-8：1.
8. the A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method according to any one of claim 1-7, its
It is characterised by, in S3, is swapped under 50-60 DEG C of water bath condition and modified 3-4h.
9. the A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method according to any one of claim 1-8, its
It is characterised by, in S3, drying temperature is 80-120 DEG C.
10. the A grades of non-combustible hydrophobic silica aerogel powder atmospheric preparation method according to any one of claim 1-9,
Characterized in that, in S4, the temperature of Muffle furnace is 320-380 DEG C, and heat treatment time is 6-7h；Preferably, in S4, Muffle
The temperature of stove is 350 DEG C, and heat treatment time is 6.5h.
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| CN109809415A (en) * | 2017-11-22 | 2019-05-28 | 台湾气凝胶科技材料开发股份有限公司 | Wet glue particle of aeroge and preparation method thereof |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621419A (en) * | 2014-12-02 | 2016-06-01 | 北京建工新型建材有限责任公司 | Ambient preparation method for silica aerogel powder |
| CN106082243A (en) * | 2016-06-12 | 2016-11-09 | 伊科纳诺（北京）科技发展有限公司 | A kind of normal pressure fast preparation method of hydrophobic silica aerogel powder body |
-
2016
- 2016-12-28 CN CN201611233827.2A patent/CN106745001A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105621419A (en) * | 2014-12-02 | 2016-06-01 | 北京建工新型建材有限责任公司 | Ambient preparation method for silica aerogel powder |
| CN106082243A (en) * | 2016-06-12 | 2016-11-09 | 伊科纳诺（北京）科技发展有限公司 | A kind of normal pressure fast preparation method of hydrophobic silica aerogel powder body |
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| CN113544091A (en) * | 2019-03-06 | 2021-10-22 | 扶桑化学工业株式会社 | Hydrophobic silica powder and toner resin particles |
| CN113683387A (en) * | 2020-05-18 | 2021-11-23 | 江苏泛亚微透科技股份有限公司 | Hydrophobic flame-retardant silicon dioxide aerogel ceramic fiber felt and preparation method thereof |
| CN112169241A (en) * | 2020-10-29 | 2021-01-05 | 安华消防新材料科技（江苏）有限公司 | Water-based aerogel efficient fire extinguishing agent and preparation method thereof |
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| CN112592149A (en) * | 2020-12-31 | 2021-04-02 | 山东大学 | Method for rapidly preparing silicon dioxide aerogel composite material by taking water glass as raw material through single solvent exchange |
| CN113562735A (en) * | 2021-08-23 | 2021-10-29 | 中南大学 | Hydrophobic silica aerogel with high thermal stability and low calorific value as well as preparation method and application thereof |
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| CN114538452A (en) * | 2022-03-15 | 2022-05-27 | 金三江(肇庆)硅材料股份有限公司 | Silica wet gel with narrow particle size distribution and preparation method and application thereof |
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| CN114804123A (en) * | 2022-04-19 | 2022-07-29 | 江苏安珈新材料科技有限公司 | Method for preparing hydrophobic silica aerogel based on aqueous solution of inorganic salt |
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| CN115012208A (en) * | 2022-06-28 | 2022-09-06 | 武汉中科先进材料科技有限公司 | Efficient normal-pressure drying large-scale preparation method of silica aerogel felt |
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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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