CN106185959B - A kind of method that aeroge is quickly prepared using microemulsion as precursor - Google Patents

A kind of method that aeroge is quickly prepared using microemulsion as precursor Download PDF

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CN106185959B
CN106185959B CN201610556529.0A CN201610556529A CN106185959B CN 106185959 B CN106185959 B CN 106185959B CN 201610556529 A CN201610556529 A CN 201610556529A CN 106185959 B CN106185959 B CN 106185959B
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microemulsion
aeroge
gel
acid
precursor
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CN106185959A (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 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
    • 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
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/155—Preparation of hydroorganogels or organogels
    • 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
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/157—After-treatment of gels
    • C01B33/158—Purification; Drying; Dehydrating
    • 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
    • C01B33/14—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
    • 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
    • C01B33/166—Preparation of silica xerogels by acidification of silicate in the presence of an inert organic phase
    • C—CHEMISTRY; METALLURGY
    • 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
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C04B14/38—Fibrous materials; Whiskers
    • C—CHEMISTRY; METALLURGY
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    • 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
    • C04B14/38—Fibrous materials; Whiskers
    • C04B14/42—Glass
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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
    • C04B24/42—Organo-silicon compounds
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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
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/10—Solid density
    • C—CHEMISTRY; METALLURGY
    • 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
    • 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 that aeroge is quickly prepared using microemulsion as precursor, including 1. measure specific water-soluble silicon source and are made into the quantitative aqueous solution, and add a certain amount of surfactant and cosurfactant, fully dissolving；2. measuring 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 and inorganic additive, fibrofelt is compound, and through certain time, form solidifying phase, through aging, normal pressure or supercritical drying, can obtain fibrofelt aerogel composite.Preparation technology of the present invention is novel, and cost of material is low, applied widely, can both use constant pressure and dry method, it is also possible to which supercritical drying process, obtained material have excellent thermal and insulating performance, and structural strength is high, and long-term use of shrinkage factor is small.

Description

A kind of method that aeroge is quickly prepared using microemulsion as precursor
Technical field
The present invention relates to a kind of method that aeroge and its composite are prepared using microemulsion as precursor, especially one kind relates to And the quick method for preparing hydrophobic aerogel and its composite of surface-hydrophobicized modification is completed in microemulsion system.
Background technology
Aerosil be it is a kind of mutually assembled by nano-scale particle form, the novel light using air as decentralized medium Matter porous material.Its hole ratio is up to 80-99%, and the typical sizes of hole are 1-100 nanometers, has that thermal conductivity factor is low, acoustic impedance Low, the advantages that refractive index is low and absorption property is strong, peculiar property is shown in chemistry, calorifics, optics, acoustics, electricity etc., Had broad application prospects in total rudder field such as Aero-Space, military project, communication, medical treatment, material, electronics, metallurgy, chemical industry. Britain in 2007《The Times》It is " the magical material that can change the world " to praise aerosil highly.
There is huge application potential just because of it, researchers all over the world put into one after another energy develop it is various Aerosil preparation method.Comprehensive existing patent and document, aerosil production method is from dry at present Constant pressure and dry and the class of supercritical drying two are broadly divided into dry mode；From silicon source species point, be broadly divided into inorganic silicon source and The major class of organic silicon source two；The modified and dry major class of post-modification two before drying is broadly divided into from the modification mode of surface.It is common Preparation flow is mainly comprising the hydrolysis of 1. silicon sources, 2. colloidal sol hydrophobizations, 3. sol-gel process（Compound other materials）, 4. gels Solvent displacement, the modification of 6. gel surfaces in aging, 5. gels（Silicic acid anhydride）, 7. drying processes（Overcritical or normal pressure is done It is dry）, 8. aeroge surface modifications（Silicic acid anhydride）.
Some steps of above procedure can not be necessary step in different technique, also have some preparation technologies to need to increase Add more intermediate steps.
Typical organosilicon silicon source preparation technology uses tetraethyl orthosilicate or methyl silicate（And corresponding polymer）For silicon source, Using the mixed liquor of ethanol or second alcohol and water as solvent, add acid and be hydrolyzed, adding alkali makes hydrolyzate accelerate gel, increases through aging By force, and with organic solvent the liquid in gel is repeatedly replaced, then passes through trim,ethylchlorosilane or HMDS, pregnancy Base disiloxane isoreactivity silane reagent carries out surface-hydrophobicized processing to gel, is then dredged through overcritical or constant pressure and dry The aerosil of aquation.Such method is raw materials used generally expensive, and has toxicity, complex process, organic solvent Dosage is big, security is relatively low, constrains the large-scale production and application of the technique.Such as patent CN101671030B, CN101264891B、US5830387、CN100384726C、CN100400153C。
Typical inorganic silicon source prepares aerosil technique and uses waterglass as silicon source, in the help of ion exchange resin Under, acidic silicasol is obtained, adding alkali makes Ludox be polycondensed into gel, then removes electrolyte using water washing gel, or By repeatedly washing after gel is formed, electrolyte is removed；Then hydrogel is repeatedly replaced with organic solvent, makes gel Interior water content is reduced to certain value, and passes through trim,ethylchlorosilane, HMDS, HMDO isoreactivity Silane reagent carries out surface-hydrophobicized processing to gel, then obtains the silica gas of hydrophobization through overcritical or constant pressure and dry Gel.Such as patent WO96/22942（CN1181053A）、WO97/17288（CN1087271C）、WO97/48642 （CN1105679C）、WO98/23367（CN1101725C）、EP-A-0658513、CN1636871B、CN1241953B、 CN101844771A.Such method is cumbersome, production cycle length, and a large amount of brine wastes can be produced in preparation technology.
Typical post-modification method, typically on the basis of above-mentioned sol-gel-aging-displacement, eliminate silanes modification The surface modification process of liquid, and after supercritical drying, by way of silylating reagent gaseous state is stifling, to aeroge surface Carry out silicic acid anhydride.Such as patent：CN1317188C, US6005012, US5738801 etc., this method would generally remain heavier The smell of silane reagent or its catabolite.
Method of modifying before typical, includes two ways：Carried out first, being soaked after gel-forming by silylating reagent Surface modification, usual organic reagent dosage is larger, and the time is longer；Another kind is i.e. from organophilic gel technique, typically in colloidal sol In process for preparation, silylating reagent is added, such as MTMS, MTES, dimethyl diethoxy Silane etc., in the presence of acid or base catalyst, these silylating reagents hydrolyze, the hydrolysis production containing hydrophobic grouping Thing interacts with sol particles caused by other silicon source hydrolysis-condensations, and hydrophobic grouping is connected to particle surface, then is urged through alkalescence Under agent effect, gel is polycondensed into, then obtains hydrophobic aerosil through drying process.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 generation, sol particles surface is largely enclosed with hydrophobic grouping, tends to cause mutually to arrange between particle Reprimand, gel process is obstructed, even if adding various base catalysts, gel process can also prolong significantly than the situation of no hydrophobic grouping Long, such as in patent CN100372765C, gel time needs more than 4 hours；The gel strength of formation is relatively weak, it is necessary to long The ageing or aging of time, need in patent CN100372765C to be aged 24h.
Also some inventors attempt in a manner of adding surfactant, modification or post-modification and solvent are transposed before avoiding Journey, such as patent CN103204666A, CN103496707A, what is obtained is the xerogel of hydrophilic either hydrophobicity difference, density Higher, porosity and specific surface area are relatively low.
To sum up, prepare that aerosil cost is higher, and consumption of organic solvent is big, security is relatively low with organic silicon source；It is inorganic Silicon source attracts attention because cheap, but still suffers from the problems such as cumbersome, the production cycle is long.It can be contracted from organophilic gel technique Short production cycle and the use for avoiding a large amount of organic reagents, but the cost of its current raw material is higher, constrains the application of the technique.
Patent CN104003406A discloses a kind of method for preparing aerogel powder, it is characterised in that：Using silicon source solution, oil Microemulsion prepared by phase, surfactant and cosurfactant prepares wet gel, is replaced through Chen Hua, washing, solvent, surface Modification, normal pressure and temperature obtain hydrophobic silicon dioxide aerogel powder after drying.This method is prepared with aforementioned inorganic silicon source The process difference of aeroge is to prepare wet gel using microemulsion method, and subsequent process is still traditional cumbersome processing side Method, consumption of organic solvent is big in washing and replacement process, longer plus surface modification treatment, whole process.
Based on this, propose the present invention.
The content of the invention
For the features and deficiency of process above in the prior art, the invention provides one kind using microemulsion as precursor The quick method for preparing aeroge, this method want raw material based on water-soluble inorganic silicon source, realize it from hydrophobic with microemulsion method Change process, effectively prevent before this from the weak point of hydrophobic technique, shorten the whole production cycle, avoid it is numerous and diverse displacement, Process of Surface Modification, the good hydrophobic silica aerogel material of resistance to elevated temperatures is obtained.
To reach above-mentioned purpose, the present invention is achieved by the following technical solutions：
A kind of method that aeroge is quickly prepared using microemulsion as precursor, it is characterised in that comprise the following steps：
（1）The preparation of microemulsion：Quantitative water-soluble silicon source is mixed with water, quantitative surfactant is added and helps table Face activating agent；Under agitator high-speed stirred, one or more organo-silicon compound and aid oil phase are slowly added to, until obtaining Translucent uniform microemulsion；
（2）The preparation of gel：By step（1）Obtained microemulsion, pass through certain time, and/or the acidity that addition is appropriate Or base catalyst accelerates gel；
（3）Aging strengthens process：By step（2）The gel rubber material of formation, within a certain period of time, and/or in heating condition Lower carry out aging；
（4）Overcritical or constant pressure and dry：By step（3）Resulting gel carries out overcritical or constant pressure and dry, is dredged The aerosil of water.
The step（1）In water-soluble silicon source be waterglass, the alkalescence that solvent is the acidic silicasol of water, solvent is water Ludox, methane-siliconic acid lithium, sodium methyl silicate, potassium methyl silicate, lithium metasilicate, lithium metasilicate, sodium metasilicate, sodium metasilicate, silicic acid One or more in potassium or potassium metasilicate；
The step（1）In surfactant for dioctyl sodium sulfosuccinate, dodecyl sodium sulfate, dodecyl Benzene sulfonic acid sodium salt, lauryl sodium sulfate, sodium sulfate of polyethenoxy ether of fatty alcohol, polysorbate60, Tween 80, span 20 or polyethylene glycol One or more in monoleate；
The step（1）In cosurfactant for acetone, espeleton, methylisobutylketone, ethyl acetate, methanol, One or more in ethanol, ethylene glycol, normal propyl alcohol or isopropanol；
The step（1）In organo-silicon compound for HMDO, HMDS, dimethyl diethyl TMOS, the hydrogen silane of monomethyl diethoxy one, MTES, MTMS, the second of poly- methyl three TMOS, poly- MTMS, methylhydroxy silicone oil, hydroxyl hydrogen silicone oil, methyl trifluoro propyl silicone oil or methyl One or more in vinyl silicone oil；
The step（1）In aid oil phase be n-hexane, hexamethylene, pentane or atoleine in one kind or more Kind.
The step（2）In acidic catalyst be hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, oxalic acid, acetic acid or ethanedioic acid in It is one or more；The step（2）In base catalyst for ammoniacal liquor, sodium hydroxide, potassium hydroxide, calcium hydroxide, hydroxide One or more in lithium, sodium carbonate or potassium carbonate.
The step（2）In addition is acid or base catalyst before, by step（1）Obtained microemulsion, add suitable The inorganic additive of amount, after being well mixed, by microemulsion spray permeate or by way of integrally submerging it is compound with fibrous material, Microemulsion is changed into after gel and forms an entirety with fiber.
Described fibrous material is glass fibre, alumina silicate fibre, mullite fiber, basalt fibre, polyester fiber, poly- One or more in Dralon, carbon fiber or viscose fiber；Described inorganic additive be titanium dioxide, iron oxide, Ferrous oxide, aluminum oxide, magnesia, zinc oxide, alumina silicate, magnesium silicate, calcium silicates, zinc silicate, Firebrake ZB, magnesium hydroxide, hydrogen One or more in aluminum oxide or iron hydroxide.
The step（3）In ageing time be 10min-10h, aging temperature is 10-75 DEG C.The step（3）It is old During change, a certain amount of organic solvent is added, described organic solvent is the one or more in methanol, ethanol or acetone.
The step（4）In, in atmospheric conditions, drying temperature is 50-200 DEG C, in CO 2 supercritical dried strip Under part, drying temperature is 30-65 DEG C；Under the conditions of ethanol supercritical drying, drying temperature is 220-250 DEG C.
The present invention compared with the conventional method, has advantages below：
1st, silicon source is wanted based on water-soluble silicon source, cost is cheap, has large-scale production prospect；
2nd, presoma is prepared using microemulsion method, has both completed hydrophobization process, can also form gel faster, reduced hydrophobic Change influence of the reagent to gel process；
3rd, operating process is succinctly quick, avoids a large amount of uses of organic reagent, shortens whole manufacturing process；
4th, method novel and unique, microemulsion method and the features of sol-gel process have fully been merged, has broken conventional gel system The single-mode of standby middle sol-gel process, new thinking is provided for the production of hydrophobic silica aerogel；
5th, microemulsion wetability, the permeability that this method is matched somebody with somebody are good, with various inorganic additives, fibrous material compatibility Well, obtained aerogel material high mechanical strength, resistance to elevated temperatures are good.
Brief description of the drawings
Fig. 1 is that the aqueous phase containing inorganic silicon source forms mutual friendship on a microscopic level with the oil phase containing organo-silicon compound Wrong 3-D solid structure figure；
Fig. 2 is aeroge micro-structure diagram produced by the present invention.
Embodiment
With reference to 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, sequentially add Water 650ml, butanedioic acid dibutyl ester sodium sulfonate 30g, acetone 20g, n-hexane 350g, MTES 150g, high-speed stirring Mix up to obtaining translucent uniform microemulsion, add a small amount of aqueous sulfuric acid, adjust pH to 8, high-speed stirred 10min, so After pour into mould, stand 40 minutes, microemulsion is transformed into translucent blue and white gel；Gel is placed in aging in 60 DEG C of ethanol 1h, by effectively sealing and add a small amount of ethanol in ageing process, prevent gel because solvent volatilizees fragmentation.After the completion of aging, Gel is placed in 150 DEG C of air dry ovens and dries 2h, that is, obtains hydrophobic silica aerogel block, density is about 110mg/ Cm3, microstructure such as stereoscan photograph are as shown in Figure 2.
2. microemulsion method prepares aeroge fibrofelt-CO 2 supercritical and dried
Waterglass 500ml, while high-speed stirred, sequentially add water 800ml, lauryl sodium sulfate 36g, ethyl acetate 20g, isopropanol 10g, n-hexane 350g, poly- MTES 200g, high-speed stirred is until obtain translucent uniform Microemulsion, adds a small amount of aqueous sulfuric acid, adjusts pH to 7, high-speed stirred 10min, stand-by.Take fiberglass needled mat one Block, long 30cm, wide 30cm, thickness 10mm, density 80kg/m3, it is laid in ready mould, the micro emulsion that then will have been configured Liquid uniformly pours into mould, until fibrofelt is saturated with liquid, covers die cover plate, prevents from volatilizing.After standing 30 minutes, glass is formed The gel rubber material of glass fiber composite；Gel rubber material is placed in aging 5h in 60 DEG C of ethanol, ethanol volume is the 5 of gel rubber material volume Times；After the completion of aging, gel rubber material is put into carbon dioxide supercritical extraction kettle, pressure 10Mpa is set, 40 DEG C of temperature, done After dry 6h, insulation decompression, hydrophobic, high intensity fibrofelt dioxide composite Silica Aerogels, 25 DEG C of heat conduction are finally given Coefficient is 0.0155W/m*K.
3. microemulsion method prepares enhanced aeroge fibrofelt-supercritical drying
Waterglass 300ml, sodium methyl silicate 200ml, while high-speed stirred, sequentially add water, 600ml, dodecyl Sodium sulphate 36g, acetone 20g, isopropanol 10g, n-hexane 300g, poly- MTES 200g, methylhydroxy silicone oil 50g, high-speed stirred add a small amount of aqueous sulfuric acid, adjust pH to 7, Ran Houjia up to obtaining translucent uniform microemulsion Enter titanium dioxide 15g, aluminium hydroxide 12g, magnesium hydroxide 12, iron hydroxide 12g, high-speed stirred 10min are stand-by.Take glass fibers Dimension with one piece, long 30cm, wide 30cm, thickness 10mm, density 100kg/m3 of mullite fiber mixing Nomex, glass fibre and The weight ratio of mullite fiber is 7:3, it is laid in ready mould, the microemulsion configured is uniformly then poured into mould Tool, until fibrofelt is saturated with liquid, die cover plate is covered, prevents from volatilizing.After standing 40 minutes, inorganic additive -- fiber is formed Compound gel rubber material；Gel rubber material is placed in aging 5h in 60 DEG C of ethanol, ethanol volume is 5 times of gel rubber material volume；Always After the completion of change, gel rubber material is put into carbon dioxide supercritical extraction kettle, pressure 12Mpa is set, temperature 50 C, dries 6h Afterwards, insulation decompression, finally gives hydrophobic, enhanced fiber composite silica aerogel material, inorganic additive disperses More uniform, 25 DEG C of thermal conductivity factors are 0.0186W/m*K, and thermal conductivity factor during 500 DEG C of mean temperature is 0.059W/m*K, 800 DEG C Lower 24 hours shrinkage factors are less than 2%, have excellent applied at elevated temperature performance.
The invention provides a kind of using microemulsion as precursor, low cost, the quick side for preparing hydrophobic aerogel and its composite Method.Microemulsion is two kinds of non soluble liquids spontaneously formed under surfactant and cosurfactant effect it is homogeneous Bright, thermodynamically stable dispersion.Two kinds of immiscible continuous medias are divided into small by surfactant parents' molecule Space forms microreactor, and its size can be controlled in nano-scale range, and reactant reacts generation solid phase particles in system.By The particle diameter and stability of nano material are accurately controlled in micro emulsion liquid energy, limit the nucleation of nano-particle, growth, poly- The processes such as knot, reunion, so as to which the nano-particle formed is enclosed with layer of surface activating agent, and there is certain condensed state structure.
The present invention is aided with high-speed stirred, by the water of water-soluble silicon source by adding surfactant and cosurfactant Solution forms uniform and stable microemulsion system with organo-silicon compound not soluble in water and aid oil phase, contains inorganic silicon source Aqueous phase forms interlaced 3-D solid structure on a microscopic level with the oil phase containing organo-silicon compound, as shown in figure 1, Surfactant then forms dynamic boundary between the two phases with cosurfactant, by certain time or passes through regulation system Acid-base value and temperature accelerate, and the inorganic silicon source in microemulsion system is gradually condensed into three-dimensional skeleton, and organosilicon simultaneously Hydroxyl that compound obtains through hydrolysis or existing and the hydroxyl on above-mentioned skeleton surface are mutually condensed, and organo-silicon compound are coated On skeleton surface.Also it can immerse fluffy fiber felt matrix before microemulsion loses flowability, be compounded to form mutually with fibrofelt The composite of enhancing.Condensation product obtained above or its composite, strengthen by further aging, can be obtained after constant pressure and dry Hydrophobic aeroge and its composite；Also it can be aided with organic solvent while aging strengthens and replace in condensation product hole Water, then obtain hydrophobic aeroge and its composite through supercritical drying.
Preparation technology of the present invention is novel, and cost of material is low, applied widely, can both use constant pressure and dry method, it is also possible to super Critical drying process, obtained material have excellent thermal and insulating performance, and structural strength is high, and long-term use of shrinkage factor is small.
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 for carrying out unsubstantiality to the present invention using this design, all should fall into protection scope of the present invention.

Claims (7)

  1. A kind of 1. method that aeroge is quickly prepared using microemulsion as precursor, it is characterised in that comprise the following steps：
    （1）The preparation of microemulsion：Quantitative water-soluble silicon source is mixed with water, quantitative surfactant is added and helps surface to live Property agent；Under agitator high-speed stirred, one or more organo-silicon compound and aid oil phase are slowly added to, until obtaining semi-transparent Bright uniform microemulsion；
    （2）The preparation of gel：By step（1）Obtained microemulsion, by certain time, and/or add appropriate acidity or alkali Property catalyst accelerate gel；
    （3）Aging strengthens process：By step（2）The gel rubber material of formation, within a certain period of time, and/or enter in a heated condition Row aging；
    （4）Overcritical or constant pressure and dry：By step（3）Resulting gel carries out overcritical or constant pressure and dry, obtains hydrophobic Aerosil；
    The step（2）In addition is acid or base catalyst before, by step（1）Obtained microemulsion, add appropriate Inorganic additive, after being well mixed, by microemulsion spray permeate or by way of integrally submerging with fibrous material compound, micro emulsion Liquid is changed into after gel and forms an entirety with fiber.
  2. 2. the method for aeroge is quickly prepared using microemulsion as precursor as claimed in claim 1, it is characterised in that：The step （1）In water-soluble silicon source be waterglass, solvent is the acidic silicasol of water, solvent is the alkaline silica sol of water, methane-siliconic acid In lithium, sodium methyl silicate, potassium methyl silicate, lithium metasilicate, lithium metasilicate, sodium metasilicate, sodium metasilicate, potassium silicate or potassium metasilicate It is one or more；
    The step（1）In surfactant for dioctyl sodium sulfosuccinate, dodecyl sodium sulfate, detergent alkylate sulphur Sour sodium, lauryl sodium sulfate, sodium sulfate of polyethenoxy ether of fatty alcohol, polysorbate60, Tween 80, span 20 or polyethyleneglycol oil One or more in acid esters；
    The step（1）In cosurfactant for acetone, espeleton, methylisobutylketone, ethyl acetate, methanol, ethanol, One or more in ethylene glycol, normal propyl alcohol or isopropanol；
    The step（1）In organo-silicon compound for HMDO, HMDS, dimethyl diethoxy Silane, the hydrogen silane of monomethyl diethoxy one, 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；
    The step（1）In aid oil phase be n-hexane, hexamethylene, pentane or atoleine in one or more.
  3. 3. the method for aeroge is quickly prepared using microemulsion as precursor as claimed in claim 1, it is characterised in that：The step （2）In acidic catalyst be hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, oxalic acid, acetic acid or ethanedioic acid in one or more；The step Suddenly（2）In base catalyst be ammoniacal liquor, sodium hydroxide, potassium hydroxide, calcium hydroxide, lithium hydroxide, sodium carbonate or potassium carbonate In one or more.
  4. 4. the method for aeroge is quickly prepared using microemulsion as precursor as claimed in claim 1, 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 the one or more in viscose fiber；Described inorganic additive is titanium dioxide, iron oxide, ferrous oxide, aluminum oxide, oxygen Change in magnesium, zinc oxide, alumina silicate, magnesium silicate, calcium silicates, zinc silicate, Firebrake ZB, magnesium hydroxide, aluminium hydroxide or iron hydroxide One or more.
  5. 5. the method for aeroge is quickly prepared using microemulsion as precursor as claimed in claim 1, it is characterised in that：The step （3）In ageing time be 10min-10h, aging temperature is 10-75 DEG C.
  6. 6. the method for aeroge is quickly prepared using microemulsion as precursor as described in claim 1 or 5, it is characterised in that：The step Suddenly（3）Ageing process in, add a certain amount of organic solvent, described organic solvent is one in methanol, ethanol or acetone Kind is a variety of.
  7. 7. the method for aeroge is quickly prepared using microemulsion as precursor as claimed in claim 1, it is characterised in that：The step （4）In, in atmospheric conditions, drying temperature is 50-200 DEG C, and under CO 2 supercritical drying condition, drying temperature is 30-65℃；Under the conditions of ethanol supercritical drying, drying temperature is 220-250 DEG C.
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