CN106185959A - A kind of method quickly preparing aeroge with microemulsion for precursor - Google Patents

A kind of method quickly preparing aeroge with microemulsion for precursor Download PDF

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CN106185959A
CN106185959A CN201610556529.0A CN201610556529A CN106185959A CN 106185959 A CN106185959 A CN 106185959A CN 201610556529 A CN201610556529 A CN 201610556529A CN 106185959 A CN106185959 A CN 106185959A
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microemulsion
precursor
described step
acid
sodium
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CN106185959B (en
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姜法兴
林芬
熊风
周水林
赵科仁
姚献东
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NANUO TECHNOLOGY Co Ltd
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NANUO TECHNOLOGY Co Ltd
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Priority to DE112017001567.7T priority patent/DE112017001567T5/en
Priority to PCT/CN2017/098237 priority patent/WO2018049965A1/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/16—Preparation of silica xerogels
    • C01B33/163—Preparation of silica xerogels by hydrolysis of organosilicon compounds, e.g. ethyl orthosilicate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0091—Preparation of aerogels, e.g. xerogels
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    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/155—Preparation of hydroorganogels or organogels
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157—After-treatment of gels
    • C01B33/158—Purification; Drying; Dehydrating
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    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157—After-treatment of gels
    • C01B33/158—Purification; Drying; Dehydrating
    • C01B33/1585—Dehydration into aerogels
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/16—Preparation of silica xerogels
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00—Silicon; Compounds thereof
    • 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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    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02—Granular materials, e.g. microballoons
    • C04B14/04—Silica-rich materials; Silicates
    • C04B14/06—Quartz; Sand
    • C04B14/064—Silica aerogel
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    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/38—Fibrous materials; Whiskers
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    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
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    • C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
    • C04B24/40—Compounds containing silicon, titanium or zirconium or other organo-metallic compounds; Organo-clays; Organo-inorganic complexes
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    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
    • C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors

Abstract

The present invention relates to a kind of method quickly preparing aeroge with microemulsion for precursor, measure specific water-soluble silicon source including 1. and be made into quantitative aqueous solution, and add a certain amount of surfactant and cosurfactant, fully dissolve；2. measure specific reactive organosilicon compounds and aid oil phase, add in above-mentioned solution, high-speed stirred certain time, form translucent uniform and stable mixed liquor, i.e. microemulsion；3. above-mentioned microemulsion is combined with inorganic additive, fiber felt, and through certain time, forms solidifying phase, through aging, normal pressure or supercritical drying, available fiber felt aerogel composite.Preparation technology of the present invention is novel, and cost of material is low, applied widely, both can use constant pressure and dry method, it is also possible to supercritical drying process, and the material obtained has excellent thermal and insulating performance, and structural strength is high, and life-time service shrinkage factor is little.

Description

A kind of method quickly preparing aeroge with microemulsion for precursor
Technical field
The present invention relates to a kind of method preparing aeroge and composite thereof for precursor with microemulsion, especially one relates to And in microemulsion system, complete the method quickly preparing hydrophobic aerogel and composite thereof of surface-hydrophobicized modification.
Background technology
Aerosil is to form a kind of mutually gathering by nano_scale particle, the Novel light with air as disperse medium Matter porous material.Its hole ratio is up to 80-99%, and the typical sizes of hole is 1-100 nanometer, has that heat conductivity is low, acoustic impedance The advantage such as low, refractive index is low and absorption property is strong, shows peculiar property at aspects such as chemistry, calorifics, optics, acoustics, electricity, Have broad application prospects in total rudder field such as Aero-Space, military project, communication, medical treatment, material, electronics, metallurgy, chemical industry. Within 2007, Britain's ' The Times ' highly praise aerosil is " the magical material that can change the world ".Have just because of it Huge application potential, researchers all over the world is had to put into energy one after another and develop various aerosil Preparation method.Comprehensive existing patent and document, current aerosil production method is broadly divided into from drying mode Constant pressure and dry and supercritical drying two class；Divide from silicon source category, be broadly divided into the big class in inorganic eka-silicon source and organic eka-silicon source two； Modified and dried modified two big classes before being dried it are broadly divided into from surface modification mode.Common preparation flow mainly comprises 1. The hydrolysis of silicon source, 2. colloidal sol hydrophobization, 3. sol-gel process (compound other materials), 4. gel be aging, 5. solvent is put in gel Change, 6. gel surface modification (hydrophobization process), 7. dry run (supercritical or constant pressure and dry), 8. aeroge surface are modified (hydrophobization process).Some step of above procedure can not be necessary step in different technique, also has some to prepare Technique needs to increase more intermediate steps.Typical organosilicon silicon source preparation technology uses tetraethyl orthosilicate or methyl silicate (and corresponding polymer) is silicon source, with the mixed liquor of ethanol or second alcohol and water as solvent, adds acid and is hydrolyzed, add alkali and make Hydrolyzed solution accelerates gel, through aging enhancing, and repeatedly replaces the liquid in gel with organic solvent, then passes through trimethylchloro-silicane Alkane or hexamethyldisiloxane, hexamethyl disiloxane isoreactivity silane reagent carry out surface-hydrophobicized process to gel, then The aerosil of hydrophobization is obtained through supercritical or constant pressure and dry.This type of method is raw materials used generally expensive, and tool Toxic, complex process, consumption of organic solvent are big, safety is relatively low, constrain large-scale production and the application of this technique.As specially Profit CN101671030B, CN101264891B, US5830387, CN100384726C, CN100400153C.Typical inorganic silicon Source is prepared aerosil technique and is used waterglass to be silicon source, with the help of ion exchange resin, obtains acid silicon molten Glue, adds alkali and makes Ludox be polycondensed into gel, then makes to wash gel with water and removes electrolyte, or passes through after forming gel Repeatedly wash, remove electrolyte；Then with organic solvent, hydrogel is repeatedly replaced, make the water content in gel be reduced to Certain value, and by trim,ethylchlorosilane, hexamethyldisiloxane, hexamethyl disiloxane isoreactivity silane reagent, gel is entered The surface-hydrophobicized process of row, then obtains the aerosil of hydrophobization through supercritical or constant pressure and dry.Such as patent WO96/ 22942(CN1181053A), WO97/17288(CN1087271C), WO97/48642(CN1105679C), WO98/23367 (CN1101725C), EP-A-0658513, CN1636871B, CN1241953B, CN101844771A.The operation of this type of method is numerous Trivial, the production cycle is long, and can produce a large amount of brine waste in preparation technology.Typical post-modification method, it is common that above-mentioned molten On the basis of glue-gel-aging-displacement, eliminate the surface modification process of silanes modification liquid, and after supercritical drying, By the way of stifling with silylating reagent gaseous state, aeroge surface is carried out hydrophobization process.Such as patent: CN1317188C, US6005012, US5738801 etc., the method would generally remain the abnormal smells from the patient of heavier silane reagent or its catabolite.
Method of modifying before typical, comprises two ways: one is to be soaked by silylating reagent to carry out after gel formation Surface is modified, and usual organic reagent large usage quantity, the time is longer；Another kind is i.e. from organophilic gel technique, it is common that at colloidal sol In process for preparation, add silylating reagent, such as MTMS, MTES, dimethyl diethoxy Silane etc., under the effect of acidity or base catalyst, these silylating reagents hydrolyze, and the hydrolysis containing hydrophobic group is produced The sol particles that thing produces with other silicon source hydrolysis-condensations interacts, and hydrophobic group is connected to particle surface, then urges through alkalescence Under agent effect, being polycondensed into gel, then drying process obtains hydrophobic aerosil.Such as patent: CN100372765C, CN100398492C, CN101372337B, WO2005/110919(CN1984843A), CN101450852A、CN101439958A、CN101973752A、US8663739B2.Such method avoids the big of organic reagent Amount uses, but before gel occurs, sol particles surface is enclosed with hydrophobic group in a large number, tends to cause between particle and mutually arranges Scolding, gel process is obstructed, even if adding various base catalyst, gel process also can prolong than the situation not having hydrophobic group significantly Long, as in patent CN100372765C, gel time needs more than 4 hours；The gel strength formed is relatively weak, needs long The ageing or aging of time, needs in patent CN100372765C to be aged 24h.Also some inventors are had to attempt to add surface activity The mode of agent, it is to avoid front modification or post-modification and solvent replacement process, such as patent CN103204666A, CN103496707A, obtains To be hydrophilic or hydrophobicity difference xerogel, density is higher, and porosity and specific surface area are relatively low.To sum up, with organic It is relatively costly that aerosil is prepared in silicon source, and consumption of organic solvent is big, safety is relatively low；Inorganic silicon source is subject to because of cheap To paying close attention to, but still suffer from the problem such as complex operation, production cycle length.The production cycle can be shortened from organophilic gel technique and avoid The use of a large amount of organic reagents, but its raw material at present is relatively costly, constrains the application of this technique.Patent CN104003406A Disclose a kind of method preparing aerogel powder, it is characterised in that: use silicon source solution, oil phase, surfactant and help table Microemulsion prepared by face activating agent is to prepare wet gel, and through Chen Hua, washing, solvent replacement, surface modification treatment, normal pressure and temperature is done Hydrophobic silicon dioxide aerogel powder body is obtained after dry.The process difference of aeroge is prepared in the method and aforementioned inorganic silicon source Being to use microemulsion method to prepare wet gel, subsequent process is still traditional loaded down with trivial details processing method, in washing and replacement process Consumption of organic solvent is big, adds surface modification treatment, and whole process is longer.Have based on this, propose the present invention.
Summary of the invention
For the features of process above in prior art and deficiency, the invention provides a kind of with microemulsion as precursor The method quickly preparing aeroge, the method, with water-soluble inorganic silicon source as primary raw material, realizes it from hydrophobic with microemulsion method Change process, effectively prevent before this from the weak point of hydrophobic technique, shorten the whole production cycle, it is to avoid numerous and diverse displacement, Process of Surface Modification, has obtained the hydrophobic silica aerogel material that resistance to elevated temperatures is good.
For reaching above-mentioned purpose, the present invention is achieved by the following technical solutions:
A kind of method quickly preparing aeroge with microemulsion for precursor, it is characterised in that comprise the following steps:
(1) preparation of microemulsion: mixed with water in quantitative water-soluble silicon source, adds quantitative surfactant and helps surface to live Property agent；Under agitator high-speed stirred, it is slowly added to one or more organo-silicon compound and aid oil phase, until obtaining semi-transparent Bright uniform microemulsion；
(2) preparation of gel: microemulsion step (1) obtained, by certain time, and/or adds appropriate acidity or alkali Property catalyst accelerate gel；
(3) aging enhancing process: gel rubber material step (2) formed, within a certain period of time, and/or enters in a heated condition Row is aging；
(4) supercritical or constant pressure and dry: the gel obtained by step (3) is carried out supercritical or constant pressure and dry, it is thus achieved that hydrophobic Aerosil.
Water-soluble silicon source in described step (1) be waterglass, solvent be the acidic silicasol of water, solvent be the alkalescence of water Ludox, methane-siliconic acid lithium, sodium methyl silicate, potassium methyl silicate, Lithium metasilicate, lithium metasilicate, sodium silicate, sodium metasilicate, silicic acid One or more in potassium or potassium metasilicate；
Surfactant in described step (1) is dioctyl sodium sulfosuccinate, dodecyl sodium sulfate, detergent alkylate sulphur Acid sodium, sodium lauryl sulphate, polyoxyethylenated alcohol sodium sulfate, polysorbate60, Tween 80, span 20 or polyethyleneglycol oil One or more in acid esters；
Cosurfactant in described step (1) be acetone, espeleton, methylisobutylketone, ethyl acetate, methanol, ethanol, One or more in ethylene glycol, normal propyl alcohol or isopropanol；
Organo-silicon compound in described step (1) are hexamethyl disiloxane, hexamethyldisiloxane, dimethyl diethoxy Silane, monomethyl diethoxy one hydrogen silane, MTES, MTMS, poly-methyl triethoxy Silane, poly-MTMS, methylhydroxy silicone oil, hydroxyl hydrogen silicone oil, methyl trifluoro propyl silicone oil or ethylene methacrylic One or more in base silicone oil；
Aid oil phase in described step (1) is one or more in normal hexane, hexamethylene, pentane or liquid paraffin.
Acidic catalyst in described step (2) is in hydrochloric acid, sulphuric acid, nitric acid, phosphoric acid, oxalic acid, acetic acid or ethanedioic acid One or more；Base catalyst in described step (2) is ammonia, sodium hydroxide, potassium hydroxide, calcium hydroxide, hydroxide One or more in lithium, sodium carbonate or potassium carbonate.
In described step (2) before adding acidity or base catalyst, the microemulsion that step (1) is obtained, add suitable The inorganic additive of amount, after mix homogeneously, is permeated microemulsion by spray or is combined with fibrous material by the way of overall submergence, Microemulsion forms an entirety with fiber after being changed into gel.
Described fibrous material is glass fibre, alumina silicate fibre, mullite fiber, basalt fibre, polyester fiber, gathers One or more in Dralon, carbon fiber or viscose fiber；Described inorganic additive be titanium dioxide, ferrum oxide, Ferrous oxide, aluminium oxide, magnesium oxide, zinc oxide, aluminium silicate, magnesium silicate, calcium silicates, zinc silicate, Firebrake ZB, magnesium hydroxide, hydrogen One or more in aluminium oxide or hydrated ferric oxide..
Ageing time in described step (3) is 10min-10h, and aging temperature is 10-75 DEG C.Described step (3) old During change, adding a certain amount of organic solvent, described organic solvent is one or more in methanol, ethanol or acetone.
In described step (4), in atmospheric conditions, baking temperature is 50-200 DEG C, at carbon dioxide supercritical fluid drying bar Under part, baking temperature is 30-65 DEG C；Under the conditions of ethanol supercritical drying, baking temperature is 220-250 DEG C.
The present invention compared with the conventional method, has the advantage that 1, is main silicon source with water-soluble silicon source, with low cost, There is large-scale production prospect；2, use microemulsion method to prepare presoma, both complete hydrophobization process, it is possible to formed faster Gel, decreases the hydrophobic reagent impact on gel process；
3, operating process is the quickest, it is to avoid a large amount of uses of organic reagent, shortens whole manufacture process；4, method is novel Uniqueness, has fully merged the features of microemulsion method and sol-gel process, has broken sol-gel in the preparation of conventional gel The single-mode of process, the production for hydrophobic silica aerogel provides new thinking；
5, the method is joined microemulsion wettability, permeability are good, good with various inorganic additives, the fibrous material compatibility, The aerogel material mechanical strength obtained is high, and resistance to elevated temperatures is good.
Accompanying drawing explanation
Fig. 1 is that the aqueous phase containing inorganic silicon source forms mutually friendship on a microscopic level with the oil phase containing organo-silicon compound Wrong 3-D solid structure figure；
Fig. 2 is the aeroge micro-structure diagram that the present invention prepares.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited to This.
1. microemulsion method constant pressure and dry prepares aeroge alkaline silica sol 500ml, while high-speed stirred, is sequentially added into Water 650ml, succinic acid dibutyl ester sodium sulfonate 30g, acetone 20g, normal hexane 350g, MTES 150g, high-speed stirring Mixing until obtaining translucent uniform microemulsion, adding a small amount of aqueous sulfuric acid, regulate pH to 8, high-speed stirred 10min, so After pour mould into, stand 40 minutes, microemulsion is transformed into translucent blue and white gel；Gel is placed in 60 DEG C of ethanol aging 1h, by effectively sealing and adding a small amount of ethanol in ageing process, prevents gel from volatilizing fragmentation because of solvent.Aging complete after, Being dried 2h in gel is placed in 150 DEG C of air dry ovens, i.e. obtain hydrophobic silica aerogel block, density is about 110mg/ Cm3, microstructure such as stereoscan photograph is as shown in Figure 2.
2. microemulsion method prepares aeroge fiber felt-carbon dioxide supercritical fluid drying
Waterglass 500ml, while high-speed stirred, is sequentially added into water 800ml, sodium lauryl sulphate 36g, ethyl acetate 20g, Isopropanol 10g, normal hexane 350g, poly-MTES 200g, high-speed stirred is until obtaining translucent uniform microemulsion Liquid, adds a small amount of aqueous sulfuric acid, regulates pH to 7, and high-speed stirred 10min is stand-by.Take fiberglass needled mat one piece, long 30cm, wide 30cm, thickness 10mm, density 80kg/m, it is laid in ready mould, then by equal for the microemulsion that configured Even pours mould into, until fiber felt is saturated with liquid, covers die cover plate, prevents volatilization.After standing 30 minutes, form glass fibers The gel rubber material that dimension is compound；Gel rubber material is placed in aging 5h in 60 DEG C of ethanol, and ethanol volume is 5 times of gel rubber material volume； Aging complete after, gel rubber material is put into carbon dioxide supercritical fluid extraction still, pressure 10Mpa is set, temperature 40 DEG C, be dried 6h After, it is incubated blood pressure lowering, finally gives fiber felt dioxide composite Silica Aerogels hydrophobic, high intensity, 25 DEG C of heat conductivitys For 0.0155W/m*K.
3. microemulsion method prepares enhancement mode aeroge fiber felt-supercritical drying
Waterglass 300ml, sodium methyl silicate 200ml, while high-speed stirred, be sequentially added into water, 600ml, lauryl sulphate acid Sodium 36g, acetone 20g, isopropanol 10g, normal hexane 300g, poly-MTES 200g, methylhydroxy silicone oil 50g are high Speed stirring, until obtaining translucent uniform microemulsion, adds a small amount of aqueous sulfuric acid, regulates pH to 7, is subsequently adding dioxy Change titanium 15g, aluminium hydroxide 12g, magnesium hydroxide 12, hydrated ferric oxide. 12g, high-speed stirred 10min, stand-by.Take glass fibre with not Coming mineral wool mixing Nomex one piece, long 30cm, wide 30cm, thickness 10mm, density is 100kg/m, glass fibre and mullite The weight ratio of fiber is 7:3, is laid in ready mould, then pours the microemulsion configured into mould uniformly, directly It is saturated with liquid to fiber felt, covers die cover plate, prevent volatilization.After standing 40 minutes, form inorganic additive--fiber composite Gel rubber material；Gel rubber material is placed in aging 5h in 60 DEG C of ethanol, and ethanol volume is 5 times of gel rubber material volume；Aging complete Cheng Hou, puts into carbon dioxide supercritical fluid extraction still by gel rubber material, arranges pressure 12Mpa, temperature 50 C, after being dried 6h, protects Temperature drop pressure, finally gives fiber composite silica aerogel material hydrophobic, enhancement mode, and inorganic additive dispersion is more equal Even, 25 DEG C of heat conductivitys are 0.0186W/m*K, and heat conductivity during mean temperature 500 DEG C is 0.059W/m*K, at 800 DEG C 24 Hour shrinkage factor, less than 2%, has excellent applied at elevated temperature performance.The invention provides a kind of with microemulsion as precursor, low one-tenth Originally, the method quickly preparing hydrophobic aerogel and composite thereof.Microemulsion is that two kinds of non soluble liquids are at surfactant And spontaneously form under cosurfactant effect transparent and homogeneous, thermodynamically stable dispersion.Two kinds of immiscible companies Continuous medium is divided into short space to form microreactor by surfactant parents' molecule, and its size can be controlled in nanoscale model Enclosing, reactant reacts generation solid phase particles in system.Owing to microemulsion can carry out essence to the particle diameter of nano material and stability Really control, limit nanoparticle nucleation, grow, coalesce, the process such as reunion, thus the nanoparticle formed is enclosed with one layer Surfactant, and have certain condensed state structure.
The present invention, by adding surfactant and cosurfactant, is aided with high-speed stirred, by the water in water-soluble silicon source Solution forms uniform and stable microemulsion system, containing inorganic silicon source with water-fast organo-silicon compound and aid oil phase Aqueous phase forms interlaced 3-D solid structure on a microscopic level with the oil phase containing organo-silicon compound, as it is shown in figure 1, Surfactant and cosurfactant form dynamic boundary the most between the two phases, through certain time or by regulation system Acid-base value and temperature are accelerated, and the inorganic silicon source in microemulsion system is gradually condensed into three-dimensional skeleton, and organosilicon simultaneously Compound is condensed mutually through the hydroxyl of hydrolysis acquisition or existing hydroxyl with above-mentioned skeleton surface, and organo-silicon compound are coated with On skeleton surface.Also can immerse fluffy fiber felt matrix, and be compounded to form mutually with fiber felt before microemulsion loses flowability The composite strengthened.Condensation substance obtained above or its composite, through further aging enhancing, can obtain after constant pressure and dry Hydrophobic aeroge and composite thereof；Also can be aided with organic solvent and replace in condensation substance hole while aging enhancing Water, then obtains hydrophobic aeroge and composite thereof through supercritical drying.
Preparation technology of the present invention is novel, and cost of material is low, applied widely, both can use constant pressure and dry method, it is also possible to super Critical drying process, the material obtained has excellent thermal and insulating performance, and structural strength is high, and life-time service shrinkage factor is little.
Above-described embodiment is only used for illustrating the inventive concept of the present invention, rather than the restriction to rights protection of the present invention, All changes utilizing this design that the present invention carries out unsubstantiality, all should fall into protection scope of the present invention.

Claims (8)

1. the method quickly preparing aeroge with microemulsion for precursor, it is characterised in that comprise the following steps:
(1) preparation of microemulsion: mixed with water in quantitative water-soluble silicon source, adds quantitative surfactant and helps surface to live Property agent；Under agitator high-speed stirred, it is slowly added to one or more organo-silicon compound and aid oil phase, until obtaining semi-transparent Bright uniform microemulsion；
(2) preparation of gel: microemulsion step (1) obtained, by certain time, and/or adds appropriate acidity or alkali Property catalyst accelerate gel；
(3) aging enhancing process: gel rubber material step (2) formed, within a certain period of time, and/or enters in a heated condition Row is aging；
(4) supercritical or constant pressure and dry: the gel obtained by step (3) is carried out supercritical or constant pressure and dry, it is thus achieved that hydrophobic Aerosil.
2. the method quickly preparing aeroge as claimed in claim 1 with microemulsion for precursor, it is characterised in that: described step (1) the water-soluble silicon source in be waterglass, solvent be the acidic silicasol of water, solvent be the alkaline silica sol of water, methane-siliconic acid In lithium, sodium methyl silicate, potassium methyl silicate, Lithium metasilicate, lithium metasilicate, sodium silicate, sodium metasilicate, potassium silicate or potassium metasilicate One or more；
Surfactant in described step (1) is dioctyl sodium sulfosuccinate, dodecyl sodium sulfate, detergent alkylate sulphur Acid sodium, sodium lauryl sulphate, polyoxyethylenated alcohol sodium sulfate, polysorbate60, Tween 80, span 20 or polyethyleneglycol oil One or more in acid esters；
Cosurfactant in described step (1) be acetone, espeleton, methylisobutylketone, ethyl acetate, methanol, ethanol, One or more in ethylene glycol, normal propyl alcohol or isopropanol；
Organo-silicon compound in described step (1) are hexamethyl disiloxane, hexamethyldisiloxane, dimethyl diethoxy Silane, monomethyl diethoxy one hydrogen silane, MTES, MTMS, poly-methyl triethoxy Silane, poly-MTMS, methylhydroxy silicone oil, hydroxyl hydrogen silicone oil, methyl trifluoro propyl silicone oil or ethylene methacrylic One or more in base silicone oil；
Aid oil phase in described step (1) is one or more in normal hexane, hexamethylene, pentane or liquid paraffin.
3. the method quickly preparing aeroge as claimed in claim 1 with microemulsion for precursor, it is characterised in that: described step (2) acidic catalyst in is one or more in hydrochloric acid, sulphuric acid, nitric acid, phosphoric acid, oxalic acid, acetic acid or ethanedioic acid；Described step Suddenly the base catalyst in (2) is ammonia, sodium hydroxide, potassium hydroxide, calcium hydroxide, Lithium hydrate, sodium carbonate or potassium carbonate In one or more.
4. the method quickly preparing aeroge as described in claim 1 or 3 with microemulsion for precursor, it is characterised in that: described step Suddenly in (2) before adding acidity or base catalyst, the microemulsion that step (1) is obtained, add appropriate inorganic additive, After mix homogeneously, being permeated by spray by microemulsion or be combined with fibrous material by the way of overall submergence, microemulsion is changed into solidifying An entirety is formed with fiber after glue.
5. the method quickly preparing aeroge as claimed in claim 4 with microemulsion for precursor, it is characterised in that: described fiber Material is glass fibre, alumina silicate fibre, mullite fiber, basalt fibre, polyester fiber, polyacrylonitrile fibre, carbon fiber Or one or more in viscose fiber；Described inorganic additive is titanium dioxide, ferrum oxide, ferrous oxide, aluminium oxide, oxygen Change in magnesium, zinc oxide, aluminium silicate, magnesium silicate, calcium silicates, zinc silicate, Firebrake ZB, magnesium hydroxide, aluminium hydroxide or hydrated ferric oxide. One or more.
6. the method quickly preparing aeroge as claimed in claim 1 with microemulsion for precursor, it is characterised in that: described step (3) ageing time in is 10min-10h, and aging temperature is 10-75 DEG C.
7. the method quickly preparing aeroge as described in claim 1 or 6 with microemulsion for precursor, it is characterised in that: described step Suddenly in the ageing process of (3), adding a certain amount of organic solvent, described organic solvent is in methanol, ethanol or acetone Plant or multiple.
8. the method quickly preparing aeroge as claimed in claim 1 with microemulsion for precursor, it is characterised in that: described step (4) in, in atmospheric conditions, baking temperature is 50-200 DEG C, and under the conditions of carbon dioxide supercritical fluid drying, baking temperature is 30-65℃；Under the conditions of ethanol supercritical drying, baking temperature is 220-250 DEG C.
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CN112897532B (en) * 2019-11-19 2022-09-20 吉林建筑大学 Silicon dioxide aerogel powder and preparation method and application thereof
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