CN104891509A - Rapid preparation method for A-grade noncombustible silica aerogel - Google Patents
Rapid preparation method for A-grade noncombustible silica aerogel Download PDFInfo
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- CN104891509A CN104891509A CN201510236100.9A CN201510236100A CN104891509A CN 104891509 A CN104891509 A CN 104891509A CN 201510236100 A CN201510236100 A CN 201510236100A CN 104891509 A CN104891509 A CN 104891509A
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Abstract
The invention relates to an A-grade hydrophobic silica aerogel and aerogel composite material and a preparation method therefor. The preparation method comprises the steps of: (1) hydrolyzing a proportioning liquid of silicate ester and methylethoxysilane with an acid catalyst in alcohol to obtain sol; (2) adding an alkali catalyst into the sol to regulate the pH value of the sol to 6-10 so as to obtain alkali sol, and then forming wet gel by the alkali sol; or compounding the alkali sol with inorganic fibers to prepare a gel fiber composite material after obtaining the alkali sol; (3) putting aged wet gel or gel fiber composite material into a CO2 supercritical device to dry, and replacing alcohol in pores with CO2 to obtain dried silica aerogel; and (4) spraying a silane compound to the surface of a dried silica aerogel or oxygel fiber composite material, and heating a body of the silica aerogel or oxygel fiber composite material to carry out hydrophobic modification, thereby obtaining noncombustible hydrophobic silica aerogel.
Description
Technical field
The present invention relates to aerogel production field, relate to the preparation method of the non-combustible silica aerogel of a kind of A level particularly and relate to the non-combustible silica aerogel product prepared by the method.
Background technology
One of aerogel ten large novel materials being described as following most potentiality, because its porosity is up to more than 90%, thermal conductivity and density are low to moderate 0.01W/m.K and 0.03g/cm
3, so have the advantage that can not reach in insulation, heat insulation, noise reduction, sound insulation etc., future is surely for energy-saving and emission-reduction are contributed share.
Aerogel is silicon source with water glass by Stanford Univ USA Kistler teaching inventive, is prepared aerogel with sol gel process for 1931, but complex process, be not applied.
The sixties in last century, the people such as Nicolaon take silicon alkoxide as presoma, obtain wet gel with sol gel process, then use supercritical drying (SCFD) technique to obtain.But the aerogel that these techniques are prepared is hydrophilic, due to a large amount of existence of surface hydroxyl, make this material be very easy to the moisture absorption, thus make condensation vapor, improve thermal conductivity, greatly reduce the major functions such as the heat insulating of aerogel.
The 80s and 90s, investigator adds silicane organism aborning and carries out hydrophobic modification modification, if publication number is listed in the patent documentation of CN101318659A to carry out hydrophobic modification modification with silicoorganic compound such as trimethylchlorosilanes to the gel complex material after aging, then carry out drying by the mode of constant pressure and dry.The object of hydrophobic modification is the effect in order to reduce gel internal capillaries power on the one hand, thus reduces the interface interaction power of hole internal solvent and air surface, and this is the step that constant pressure and dry gel must carry out; Form hydrophobic layer on the other hand, heat preservation and soundproof effect is reduced to stop the immersion of moisture in use procedure, although aerogel prepared by this technique is provided with hydrophobic effect, but because hydrophobic modification modification is carried out in a solvent, facts have proved that must ensure the amount that organic silicon compound exceedes total mass more than 10% is attached on bulk material, just can realize most kapillary hydrophobic and be unlikely to subside.So exactly cause the Use out of range of organic compound, cause environmental pollution on the one hand, the more important thing is that so a large amount of organism at high temperature can burn, cannot reach Ministry of Public Security's public affairs to disappear the requirement of 2011 No. 65 literary compositions (" notice of requirement of having the right about further clear and definite covil construction lagging material fire supervision management "), this notice request covil construction heat insulating material for external adopts combustionproperty literary composition A level material.(GB8624-2012 " material of construction and product burns grading performance "), can say without any advantage compared with the B level material such as extruded sheet, especially under the quite severe overall situation of energy-conserving and environment-protective situation.
In the aerogel porous material preparation method that the patent documentation of publication No. CN103524111A is listed, introduce silicoorganic compound solution before it is dried equally, owing to containing a large amount of hydroxyls in wet gel, need a large amount of silane compounds could realize the object of hydrophobically modified.Although the aerogel material therefore prepared has hydrophobicity, because organic compound content exceeds standard, A level non-combustible material standard cannot be reached, therefore cannot widely use in building exterior wall heat preserving industry, limit promoting the use of of aerogel.
Summary of the invention
Cannot reach the problem of A level non-combustible material standard in view of existing aerogel hydrophobically modified, the invention provides the preparation method of a kind of A level hydrophobic aerogel and aerogel composite, the method comprises the steps:
(1) silicon ester and methylethoxy base silane proportioning liquid are fully hydrolyzed with acid catalyst in alcohol, obtain colloidal sol.
(2) in colloidal sol, add alkaline catalysts, pH value is adjusted to 6-12, the weakly acidic pH obtained or the colloidal sol of alkalescence form wet gel subsequently; Or after obtaining the colloidal sol of weakly acidic pH or alkalescence, by the colloidal sol of weakly acidic pH or alkalescence and inorganic fibre compound, prepare gelled fibre matrix material; By the wet gel obtained or or gelled fibre matrix material carry out ageing.
(3) wet gel after ageing or gelled fibre matrix material are placed in the overcritical device of CO2 and carry out drying, displace the alcohol in hole with CO2, obtain dry silica aerogel.
(4) silane compound is sprayed onto dry silica aerogel or the surface of oxygen gelled fibre matrix material, and the body of heated oxide silica aerogel or gelled fibre matrix material carries out hydrophobically modified, obtains non-combustible silica aerogel.
Further, the proportioning of the alcohol in step (1), silicon ester, methylethoxy base silane is (mass fraction) 10-20 part: 0.2-5 part: 0.2-5 part; Wherein said alcohol is the alcohol of content more than 90%.
Further, the methylethoxy base silane in step (1) is Union carbide A-162, diformazan diethoxy silane, trimethylethoxysilane or their mixture.
Further, the described silicon ester of step (1) is a kind of in methyl silicate, tetraethoxy, butyl silicate or their mixture; Described alcohol liquid is a kind of in methyl alcohol, ethanol, propyl carbinol, Virahol or their mixture; Described acid catalyst is a kind of in hydrochloric acid, sulfuric acid, acetic acid, butyric acid, formic acid or their mixture; Described alkaline catalysts is a kind of in sodium hydroxide, potassium hydroxide, ammoniacal liquor, Monoethanolamine MEA BASF, diethanolamine, trolamine or its mixture; Described silane compound is a kind of in trimethylchlorosilane, hexamethyldisilazane, hexamethyldisilazane or its mixture.
Further, hydrolysis reaction is carry out between 1-4 in pH value.
Further, in step (2), described inorganic fibre is a kind of in glass fibre, quartz glass fibre, boron fibre, ceramic fiber and steel fiber or their mixture.
Further, in step (2), wet gel or gel and fibre composite leave standstill aging 3-24 hour at the temperature of 25-70 DEG C.
Further, in step (4), the silane compound being sprayed onto the surface of dry silica aerogel or oxygen gelled fibre matrix material accounts for the 0.5-1.5% (w/w) of silica aerogel or oxygen gelled fibre composite body quality.
Further, the temperature of the hydrophobically modified in step (4) is between 50-100 DEG C.
The present invention also provides a kind of aerogel of obtaining according to above-mentioned preparation method or aerogel fibre composite.
The principal feature of the inventive method is rearmounted for hydrophobically modified step (after namely hydrophobically modified step is placed on aerogel drying, and unconventional modification wet gel), the gel body of modification or gelled fibre composite body are that dried inside has certain hydrophobic grouping but the aerosil that hydrophobic angle is less, oh group through dried aerogel surface significantly reduces, recycling silane compound spraying modification, operating weight can reach the effect of hydrophobically modified than the silane compound less than 1.5%, the organic content of inorganic oxide silica aerogel is made to reach minimum limit, not only hydrophobic organic but also the effect do not exceeded standard can be reached completely.
The silicon ester proportioning liquid of Ethoxysilane compounds (Union carbide A-162, dimethyldiethoxysilane, trimethylethoxysilane) and mass fraction 0.2-5 part that colloidal sol configuration phase of the present invention employs mass fraction 0.2-5 part is hydrolyzed.Because the former is with certain methyl hydrophobic grouping, so a small amount of hydrophobic bond can be formed, for good inner base has successfully been laid in the hydrophobic modifier modification below by minute quantity in gel inside.
The modification mode of aerogel of the present invention or gelled fibre matrix material has innovation greatly.Prior art is all after wet gel ageing or does not carry out ripening and introduce silane compound solution immediately and carry out finishing or hydrophobically modified, and the present invention carries out hydrophobically modified after the drying, like this in suitability for industrialized production with regard to condition of providing convenience for the variation of product, the words of hydrophilic product if necessary, sale can be packed, as needed hydrophobic product, then send into modification facility immediately and carry out modification; Conventional hydrophobic modification mode adopts immersion form, and hydrophobizing agent consumption is large, and adopt now spray pattern to be directly sprayed onto aerogel surface, consumption decreases a lot.
In addition, preparation method of the present invention can save the consumption of properties-correcting agent greatly.Prior art carries out modification on wet gel, owing to containing alcoholic solution hydroxyl in a large number in wet gel, silane compound has a great deal of with the hydroxyl generation substitution reaction in alcoholic solution, the several times even silane compound of more than ten times can be wasted like this, from 20000-40000 unit per ton not etc., the consumption of properties-correcting agent is directly connected to the cost of aerogel finished product for the price of silane compound.The present invention selects dry aerogel modification, only uses a small amount of silane compound (0.5-1.5% of this weight of aerogel) to complete hydrophobically modified.
Preparation method of the present invention can greatly reduce organic compound content, and reach the non-combustible standard of A level, environmental protection is safety again.
Accompanying drawing explanation
Fig. 1 illustrates the Hydrophobic silica aerogel prepared by method of the present invention.
Fig. 2 illustrates the Hydrophobic silica aerogel blanket prepared by method of the present invention.
Fig. 3 illustrates the Electronic Speculum figure being prepared aerogel by method of the present invention.
Embodiment
Embodiment 1
Extract the industrial methanol 500 grams of 90-95% content, the pH regulator of system is 1 by the aqueous hydrochloric acid of instillation 1wt% concentration.After stirring, at the uniform velocity instill methyl silicate (99%wt) 150 grams and Union carbide A-162 50 grams of mixed solutions, and at the uniform velocity after stir about 10-40 minute, instill the aqueous sodium hydroxide solution heightening pH value of 1% concentration, stir, leave standstill after 10-60 minute, namely form gel.Environment gel being placed in 50 DEG C can carry out supercritical drying after aging 5 hours.Aging good gel be placed in autoclave and close, in autoclave, slowly injecting liquid CO
2, and about 60 DEG C will be warming up in still, now still internal pressure can rise to 10-15MPa, within the scope of this temperature and pressure, use CO
2methyl alcohol in displacement still, by near for methanol content in still less than 0.1% after about 4-6 hour, starts to discharge CO at a slow speed
2, namely supercritical drying completes and prepares aerogel particle, then takes out that aerogel particle is weighed, hydrophobicity and thermal conductivity detect, and detected result is: quality is 55 grams, aerogel particle is slightly hydrophilic, 25 DEG C time thermal conductivity be 0.0158W/m.K.
Aerogel particle abovementioned steps prepared is contained in beaker, the trimethylchlorosilane properties-correcting agent getting aerogel quality 1% is contained in spray kettle, by silane modifier even spraying to aerogel body surface, then beaker is closed, then airtight beaker is put into baking oven, temperature is adjusted to 85 DEG C, heating 2-4 hour, then aerogel particle is taken out, weigh, hydrophobicity, thermal conductivity and incendivity test, result shows: 55.66 grams (quality increases by 1.2%), aerogel particle is completely hydrophobic, thermal conductivity is 0.0162W/m.K, incendivity test result is that A level is non-combustible.
Embodiment 2
Preparation of sol-gel: the industrial methanol 500 grams extracting 90-95% content, the acetic acid aqueous solution of instillation 10wt% concentration, by the pH regulator of system to 4.After stirring, at the uniform velocity instill methyl silicate (99%wt) 150 grams and Union carbide A-162 50 grams of mixed solutions, and at the uniform velocity after stir about 10-40 minute, instill the aqueous sodium hydroxide solution heightening pH value to 8 of 1% concentration, stir and be namely prepared into silicon sol, silicon sol is injected length and width are thick to be respectively: the fibre glass chopped stand mat of 20cm, 20cm and 1cm, leave standstill after 10-60 minute, namely make gel glass blanket.Environment gel glass blanket being placed in 50 DEG C can carry out supercritical drying after aging 5 hours.
Supercritical drying: aging good gel glass blanket be placed in autoclave and close, inject liquid CO in autoclave
2, will be warming up to about 60 DEG C in still, now still internal pressure rises to 10-15MPa, keep, within the scope of this temperature and pressure, using CO
2replace methyl alcohol in still, after about 4-6 hour, in still within methyl alcohol surplus 0.1%, start to discharge CO at a slow speed
2, namely prepare aerogel glass composite blanket, after tested, this blanket is hydrophilic blanket, and thermal conductivity when 25 DEG C is 0.0175W/m.K.
Hydrophobically modified: the hexamethyldisilazane properties-correcting agent getting aerogel glass blanket quality 1.5% is contained in spray kettle, and be evenly sprayed on dried aerogel composite blanket surface, then beaker is closed, then airtight beaker is put into baking oven, temperature is adjusted to 95 DEG C, heating 2-4 hour, then aerogel glass composite blanket is taken out, do the test of hydrophobicity, thermal conductivity and incendivity, result shows: aerogel glass composite blanket is completely hydrophobic, thermal conductivity when 25 DEG C is 0.0181W/m.K, and incendivity test result is that A level is non-combustible.
Claims (10)
1. a preparation method for Hydrophobic silica aerogel and aerogel composite, the method comprises the steps:
(1) silicon ester and methylethoxy base silane proportioning liquid are hydrolyzed with acid catalyst in alcohol, obtain colloidal sol;
(2) in colloidal sol, add alkaline catalysts, pH value is adjusted to 6-12, the colloidal sol obtaining weakly acidic pH or alkalescence forms wet gel subsequently; Or after obtaining the colloidal sol of weakly acidic pH or alkalescence, by the colloidal sol of weakly acidic pH or alkalescence and inorganic fibre compound, prepare gelled fibre matrix material; Then, by the wet gel obtained or or gelled fibre matrix material carry out ageing;
(3) wet gel after ageing or gelled fibre matrix material are placed in CO
2carry out drying in overcritical device, use CO
2displace the alcohol in hole, obtain dry silica aerogel;
(4) silane compound is sprayed onto dry silica aerogel or the surface of oxygen gelled fibre matrix material, then the body of heated oxide silica aerogel or aerogel fibre composite carries out hydrophobically modified, obtains non-combustible Hydrophobic silica aerogel or aerogel composite.
2. preparation method according to claim 1, is characterized in that, the proportioning of the alcohol in step (1), silicon ester, methylethoxy base silane is 10-20 part by weight: 0.2-5 part: 0.2-5 part; Wherein said alcohol is the alcohol of content more than 90%.
3. preparation method according to claim 1, is characterized in that, the methylethoxy base silane in step (1) is Union carbide A-162, diformazan diethoxy silane, trimethylethoxysilane or their mixture.
4. preparation method according to claim 1, is characterized in that, the described silicon ester of step (1) is a kind of in methyl silicate, tetraethoxy, butyl silicate or their mixture; Described alcohol liquid is a kind of in methyl alcohol, ethanol, propyl carbinol, Virahol or their mixture; Described acid catalyst is a kind of in hydrochloric acid, sulfuric acid, acetic acid, butyric acid, formic acid or their mixture; Described alkaline catalysts is a kind of in sodium hydroxide, potassium hydroxide, ammoniacal liquor or their mixture; Described silane compound is a kind of in trimethylchlorosilane, hexamethyldisilazane, hexamethyldisilazane or its mixture.
5. preparation method according to claim 1, is characterized in that, the pH value of the described hydrolysis in step (1) is between 1-4.
6. preparation method according to claim 1, is characterized in that, in step (2), described inorganic fibre is a kind of in glass fibre, quartz glass fibre, boron fibre, ceramic fiber and steel fiber or their mixture.
7. preparation method according to claim 1, is characterized in that, in step (2), wet gel or gel and fibre composite leave standstill aging 3-24 hour at the temperature of 25-70 DEG C.
8. preparation method according to claim 1, it is characterized in that, in step (4), the silane compound being sprayed onto the surface of dry silica aerogel or oxygen gelled fibre matrix material accounts for the 0.5-1.5% (w/w) of silica aerogel or oxygen gelled fibre composite body quality.
9. preparation method according to claim 1, is characterized in that, the temperature of the hydrophobically modified in step (4) is between 50-100 DEG C.
10. the aerogel that obtains of the preparation method according to above any one of claim 1-9 or aerogel fibre composite.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106745002A (en) * | 2016-12-28 | 2017-05-31 | 伊科纳诺（北京）科技发展有限公司 | A kind of method that co-precursor method constant pressure and dry prepares block aerosil |
| CN107098354A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of preparation method from hydrophobic silicon hydrochlorate aerogel material |
| EP3284721A4 (en) * | 2016-03-08 | 2018-05-09 | LG Chem, Ltd. | Method for manufacturing aerogel blanket, and aerogel blanket manufactured thereby |
| CN113750914A (en) * | 2021-08-05 | 2021-12-07 | 华东理工大学 | Silicon dioxide aerogel modification method |
| CN113828505A (en) * | 2021-10-20 | 2021-12-24 | 河北金纳科技有限公司 | Method for rapidly preparing hydrophobic aerogel composite felt |
| CN116876097A (en) * | 2023-07-20 | 2023-10-13 | 中国人民解放军海军工程大学 | Polysiloxane aerogel fiber and preparation method thereof |
| CN116983914A (en) * | 2023-06-21 | 2023-11-03 | 广东埃力生科技股份有限公司 | Hydrophobic aerogel material, preparation method thereof and heat insulation material |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098354A (en) * | 2016-02-20 | 2017-08-29 | 金承黎 | A kind of preparation method from hydrophobic silicon hydrochlorate aerogel material |
| EP3284721A4 (en) * | 2016-03-08 | 2018-05-09 | LG Chem, Ltd. | Method for manufacturing aerogel blanket, and aerogel blanket manufactured thereby |
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| CN113750914A (en) * | 2021-08-05 | 2021-12-07 | 华东理工大学 | Silicon dioxide aerogel modification method |
| CN113750914B (en) * | 2021-08-05 | 2023-02-14 | 华东理工大学 | Silicon dioxide aerogel modification method |
| CN113828505A (en) * | 2021-10-20 | 2021-12-24 | 河北金纳科技有限公司 | Method for rapidly preparing hydrophobic aerogel composite felt |
| CN116983914A (en) * | 2023-06-21 | 2023-11-03 | 广东埃力生科技股份有限公司 | Hydrophobic aerogel material, preparation method thereof and heat insulation material |
| CN116876097A (en) * | 2023-07-20 | 2023-10-13 | 中国人民解放军海军工程大学 | Polysiloxane aerogel fiber and preparation method thereof |
| CN116876097B (en) * | 2023-07-20 | 2024-04-19 | 中国人民解放军海军工程大学 | Polysiloxane aerogel fiber and preparation method thereof |
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