CN103396086A - Preparation method for glass fiber-reinforced water glass-based silica composite aerogel - Google Patents
Preparation method for glass fiber-reinforced water glass-based silica composite aerogel Download PDFInfo
- Publication number
- CN103396086A CN103396086A CN2013103431194A CN201310343119A CN103396086A CN 103396086 A CN103396086 A CN 103396086A CN 2013103431194 A CN2013103431194 A CN 2013103431194A CN 201310343119 A CN201310343119 A CN 201310343119A CN 103396086 A CN103396086 A CN 103396086A
- Authority
- CN
- China
- Prior art keywords
- preparation
- silicon dioxide
- composite aerogel
- water glass
- solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention provides a preparation method for a glass fiber-reinforced water glass-based silica composite aerogel, which relates to a silica aerogel. The preparation method comprises the following steps: mixing methoxysilane with a water glass solution and water and allowing methoxysilane to be hydrolyzed in water to obtain solution A; then adding a strongly acidic styrene resin for ion exchange, carrying out pumping filtration to obtain a solution with a pH value of 2 to 3, adding a glass fiber having undergone heat treatment into the solution obtained after pumping filtration and adding ammonia water to adjust a pH value to 8 to 8.5 so as to obtain a fiber compounded silica sol; transferring the fiber compounded silica sol to a container for standing so as to obtain a composite silica hydrogel; and then immersing the composite silica hydrogel in an absolute ethyl alcohol solution for aging and alcoholization of the gel, immersing the wet gel obtained after alcoholization in a mixed solution of trimethylchlorosilane, absolute ethyl alcohol and hexane, carrying out surface modification and drying the modified gel so as to obtain the glass fiber-reinforced water glass-based silica composite aerogel. The preparation method provided by the invention has the advantages of low cost, simple process, a short production period, a controllable product shape and capacity of realizing continuous production.
Description
Technical field
The present invention relates to a kind of aerosil, especially relate to a kind of take service water glass as raw material, adopt unique twice-modified method also by quick solvent replacing, constant pressure and dry prepares glass fibre and strengthens the preparation method of water glass base silicon dioxide composite aerogel.
Background technology
Silicon-dioxide (SiO
2) aerogel is a kind of solid-phase particle, the particle pore size is the novel porous functional materials of nanometer scale, and continuous three-dimensional net structure can be controlled and cut out at nanoscale.Aerosil has the performance of many uniquenesses, and as high-specific surface area, high porosity, high thermal insulation, low density, ultralow dielectric and low specific refraction etc., performance can have continuous adjustability along with the control to its structure.The excellent properties that aerosil has makes it to have broad application prospects in fields such as heat-insulation and heat-preservation, thermal isolation, aerospace, catalyzer and carrier thereof, energy-conserving and environment-protective, petrochemical complex, drug release.
At present, the subject matter that faces of aerosil industrialization mainly comprises: complicated process of preparation, preparation cycle is long, solvent-oil ratio is large, the high-risk severe condition of supercritical drying, silicon source presoma is expensive, aerogel intensity is low, easily cracked etc.Wherein, the aerosil of constant pressure and dry preparation has the performance very approaching with the aerosil of supercritical drying preparation, but the silicon source presoma that adopts concentrates on the organosilicon presomas such as tetraethyl orthosilicate (TEOS), positive quanmethyl silicate (TMOS) substantially, this eka-silicon source presoma is expensive, and has the problem of environmental protection and safety in preparation and use procedure.And water glass due to cheap, reserves abundant, pollution-free, the advantage such as be widely used becomes the desirable silicon source for preparing aerosil.But, the water glass of using faces the preparation process complexity as the silicon source presoma of aerosil, in building-up process, each solvent-oil ratio is large, and the aerosil performance of the aerogel that makes and the preparation of estersil class presoma also has a certain distance, and aerogel is cracked more serious.The applicant reported in Chinese patent CN102897779A a kind of take water glass as the silicon source under constant pressure and dry fast, cheapness prepares the method for aerosil, the aerogel that obtains has excellent porous performance, its porosity can reach 95%, and density is 0.1～0.15g/cm
3, specific surface area is 500～800m
2/ g, perforate pore volume are 2.6～3.6cm
3/ g, contact angle are 140～150 °.But the aerosil globality of preparation is poor, and intensity is low.
At present, silicon dioxide composite aerogel is take estersil class presoma as the silicon source substantially, by sol-gel, aging, modification, drying and other steps, makes.
Publication number provides a kind of preparation method of aerogel heat-insulating composite material for the Chinese patent of CN101439957A.The method is mainly that infrared light screening agent titanium dioxide, fortifying fibre are mixed with silicon dioxide gel, then by Infiltration Technics, immerses in fiber preform, and last supercritical drying obtains aerogel composite.The composite aerogel that the method obtains has heat-proof quality preferably, but preparation cost is expensive, and adopts the supercritical drying with certain risk in technique, is unfavorable for industrialization and commercial applications.
Publication number provides a kind of preparation method who contains the composite absorption filtering material of porous aerogel for the Chinese patent of CN1861250A.The method is mainly to carry out surface modification and solvent replacing after the silica wet gel of preparation is smashed to pieces, then fiber or fabric are mixed with it, obtains the composite absorption filtering material of porous finally under constant pressure and dry.This composite aerogel has good Adsorption Filtration Properties, but is compression molding, and in composite aerogel, aerosil is Powdered, and it is only also that the mutual of physics mixes with the compound of fiber, and the porous performance remains further to be improved.
Publication number provides a kind of preparation method of the composite aerogel take the fibrous lofted tire as strongthener for the Chinese patent of CN1592651A.The method is mainly that one or more layers pre-woven batts is immersed in silicon dioxide gel, then obtains the composite aerogel of low heat conductivity by modifying and decorating or supercritical drying.Yet the batts that strengthens needs complicated craft woven to reticulate, and aerogel is combined and is made the bonding strength of matrix material limited with the filling type of batts.
The applicant provides one in the Chinese patent of publication number for CN101973752A in, glass fibre strengthens the method for aerosil.This invention, take TEOS as raw material, after the glass fibre of silanization pretreatment is added silicon sol, makes both abundant combinations by stirring, then passes through the steps such as gel and aging, modification, solvent replacing, prepares strongthener under constant pressure and dry., though the method has prepared complete composite aerogel, process complicated process of preparation but need to carry out silanization to glass fibre.
All with estersil class presoma, prepare silicon dioxide composite aerogel in the patent of above report, this will limit the industrialization of such composite aerogel greatly.In addition, the importance that is hydrolyzed in building-up process due to silicone grease class presoma, need accurately to control the proportioning, pH value of solution etc., makes the preparation susceptible to of composite aerogel.
Publication number provides a kind of brucite fiber to strengthen the preparation method of aerosil lagging material for the Chinese patent of CN1803602A.It is raw materials that this patent adopts cheap water glass, the brucite staple fibre after high-energy ball milling and chemical dispersion is scattered in silicon dioxide gel, then by solvent exchange, hydrophobically modified, prepares composite aerogel under constant pressure and dry.The strongthener brucite fiber need to be through more complicated processing in the method, and preparation technology also relates to more solvent consumption, and the material property that obtains remains further to be optimized.
Publication number provides the preparation method of a kind of aerosil/inorganic cotton composite thermal insulation felt for the Chinese patent of CN102701700A, this patent is take service water glass as presoma, by ion-exchange, with the mutual compound and gel of glass wool, again the composite aerogel block is carried out ageing and modification, prepare aerosil/glass wool composite block under constant pressure and dry.The density of this material is 0.1～0.3cm
3/ g, thermal conductivity are 0.01～0.029Wm
-1℃
-1But it is compound that the silicon sol after the exchange of preparation process intermediate ion is only undertaken by the absorption of glass wool, greatly affected homogeneity and the intensity of material, and needed the multistep modification, causes the consumption waste of properties-correcting agent and other solution and the time of preparation flow to increase.Publication number also provides the preparation method of a kind of aerogel/light inorganic collection theremal-preserving heat-insulating material for the Chinese patent of CN102795826A.Take water glass as the silicon source, after compound with various light inorganic collection sheet materials, obtain composite aerogel by supercritical drying or constant pressure and dry, in this composite heat-insulated material, the mass ratio of light inorganic collection sheet material and aerosil is 20～70: 1, has obviously improved the heat-proof quality of material.In the method, the preparation method of aerogel and relative content still need further to improve.
Summary of the invention
The object of the present invention is to provide a kind of with low cost, technique is simple, with short production cycle, shape of product is controlled, and the glass fibre that can be continuously produced strengthens the preparation method of water glass base silicon dioxide composite aerogel.
The present invention includes following steps:
1) the methyl TMOS mixed and stirs with water glass solution and deionized water, the methyl TMOS is hydrolyzed in deionized water, obtaining solution A;
2) solution A of step 1) preparation is added strongly acidic styrene's resin, carry out again ion-exchange, then suction filtration obtains the solution of pH=2～3, the solution that adds suction filtration to obtain in the glass fibre after thermal treatment, adding ammoniacal liquor regulation system pH value is 8～8.5 again, obtain the silicon dioxide gel of fiber composite, then transfer in container standingly, namely make compound silica hydrogel;
3) with step 2) the compound silica hydrogel that obtains is immersed in ethanol solution and carries out the aging of gel and alcoholization, after refining, the wet gel of gained is immersed in the mixing solutions of trimethylchlorosilane (TMCS), dehydrated alcohol and normal hexane again, carry out surface modification, gel drying after modification, obtain glass fibre and strengthen water glass base silicon dioxide composite aerogel, prepared glass fibre strengthens water glass base silicon dioxide composite aerogel and is transparent block shape.
In step 1), described methyl TMOS can adopt Union carbide A-162 (MTES) or methyltrimethoxy silane (MTMS); Press material molar ratio, water glass solution: the methyl TMOS: deionized water can be (0.8～1.2): (0.2～0.6): (30～40), and the time of described stirring can be 24～48h;
In step 2) in, by volume, the solution A of step 1) preparation: strongly acidic styrene's resin can be (0.5～2): 1, and the described front preferably standing 5～20min of ion-exchange that carries out; Described heat treated temperature can be 120～200 ℃, and the heat treated time can be 12～24h; Describedly transfer to the time standing in container and can be 10～30min.
In step 3), by volume, described ethanol solution: compound silica hydrogel can be (1.2～2): 1, and described temperature aging and that refine can be 25～60 ℃, and the time aging and alcoholization can be 24～48h; After described will the alcoholization, the wet gel of gained is immersed in the mixing solutions of trimethylchlorosilane (TMCS), dehydrated alcohol and normal hexane, can soak under air-proof condition 1～2 day; By volume, trimethylchlorosilane: dehydrated alcohol: normal hexane can be (1～3): (1～3): (6～8); The technical process of described drying is preferably: the gel after modification is incubated 6～8h at 45～50 ℃, be warming up to 65～70 ℃, be incubated again 6～8h, and then be warming up to 120 ℃, be incubated again 4～6h, be warming up to finally 200 ℃, then be incubated 4～8h, stove is chilled to room temperature subsequently, and whole drying process heat-up rate can be 1～5 ℃/min.
The porosity that prepared glass fibre strengthens water glass base silicon dioxide composite aerogel is 90%～96%, and density is 0.1～0.2g/cm
3, specific surface area is 600～800m
2/ g, hydrophobic angle is 145～155 °, aperture concentrates on 2～50nm.
the present invention is take the service water glass of cheapness as silicon source presoma, Union carbide A-162 (MTES) or methyltrimethoxy silane (MTMS) are co-precursor properties-correcting agent, after ion exchange resin treatment, take the glass fibre of sample total mass 1%～15% as reinforcement, prepare hydrogel take ammoniacal liquor as catalyzer, carry out aging in ethanol solution and one the step solvent replacing after, wet gel is at trimethylchlorosilane (TMCS), carry out surface modification in the mixing solutions of dehydrated alcohol and normal hexane, slowly heat up under air atmosphere finally, constant pressure and dry makes the dioxide composite silica aerogel.Raw material of the present invention is cheap, easily obtains, and in preparation process, solvent and properties-correcting agent consumption are few, and whole process is easy to control, and the product physicals and the good mechanical performance that obtain, can be continuously produced.
Compared with the prior art, the present invention has following outstanding advantages:
The present invention adopts twice-modified method constant pressure and dry to prepare glass fibre enhancing water glass base silicon dioxide composite aerogel, both kept the excellent properties of aerogel in the matrix material, glass fibre disperse simultaneously is distributed in the aerogel matrix, in the process of polycondensation gel, be cross-linked with each other by Si-O-Si bonding and gel substrate, strengthened gel skeleton, made composite aerogel have very little volumetric shrinkage when constant pressure and dry, the aperture of aerogel and pore volume all have significant increase; The compound expansion that suppresses aerogel crackle when constant pressure and dry of fiber, can obtain into piece composite aerogel preferably simultaneously.
That the present invention has is cheap, solvent and the characteristics such as the properties-correcting agent consumption is few, excellent product performance.Simultaneously by the compound method of glass fibre, aerosil intensity difference, fragility aerogel large, that constant pressure and dry obtains have effectively been improved irregular cracked and can't be as the shortcoming of independent block materials practical application.The water glass base silicon dioxide composite aerogel that glass fibre strengthens has obviously improved the mechanical property of material, material monolithic is better, can make more as requested the composite aerogel block materials of desired shape in actual applications, the composite felt class materials such as fibrefelt have been overcome to the synthetic single shortcoming of composite aerogel shape, and the content of glass fibre is much smaller than the content of aerosil in composite aerogel, overcome the low shortcoming of aerogel content in present composite aerogel, the advantage of utilizing the aerosil special performance has been had larger meaning.
Technical scheme of the present invention is to prepare on the basis of water glass base aerosil at constant pressure and dry, and the method by fiber composite prepares the silicon dioxide composite aerogel block.Glass fibre is reinforcement, and content is 1%～15% of sample total mass, and aerosil is matrix, and cheap water glass is silicon source material, and organoalkoxysilane (MTES or MTMS) is silicon source co-precursor, and trimethylchlorosilane (TMCS) is properties-correcting agent.
The preparation method of fiber-reinforcement silicon dioxide composite aerogel of the present invention is in air atmosphere, and the atmospheric low-temperature dry heat is carried out under processing.Prepare at constant pressure and dry on the basis of water glass base aerosil, with the organoalkoxysilane (MTES or MTMS) after hydrolysis with carry out ion-exchange after water glass mixes, then in the silicon sol after the glass fibre after with thermal treatment adds ion-exchange in the sol-gel stage, by stirring, glass fibre is dispersed in sol system, makes the water glass base silicon dioxide composite aerogel that glass fibre strengthens after gel formation is by overaging, alcoholization, modification, drying and other steps.
Description of drawings
Fig. 1 is the photo of the fiber-reinforcement silicon dioxide composite aerogel of the different shape for preparing of the present invention.(a) being block, (b) being strip, is (c) tubulose, is (d) coniform.
Fig. 2 is the N of the fiber-reinforcement silicon dioxide composite aerogel of the embodiment of the present invention 1 preparation
2Adsorption desorption isothermal curve figure.In Fig. 2, X-coordinate is relative pressure (P/P
0); Ordinate zou is adsorption volume (cm
3/ g).
Fig. 3 is the graph of pore diameter distribution of the fiber-reinforcement silicon dioxide composite aerogel of the embodiment of the present invention 1 preparation.In Fig. 3, X-coordinate is aperture (nm); Ordinate zou is pore volume (cm
3/ g).
Fig. 4 is the infrared spectrogram of the fiber-reinforcement silicon dioxide composite aerogel of the embodiment of the present invention 1 preparation.In Fig. 4, X-coordinate is wave number (cm
-1); Ordinate zou is transmitance (%).Yi Wei – CH of the chemical bond that from left to right marks
3， – CH
2, Si – O – Si, Si – C, Si – O – Si, Si – O – Si.
Fig. 5 is the scanning electron microscope (SEM) photograph of the fiber-reinforcement silicon dioxide composite aerogel of the embodiment of the present invention 1 preparation.
Fig. 6 is the contact angle figure of the fiber-reinforcement silicon dioxide composite aerogel of the embodiment of the present invention 1 preparation.
Embodiment
The invention will be further described in connection with accompanying drawing for following examples.
Embodiment 1
Material molar ratio is: water glass: MTES: water=1: 0.3: 35, MTES with 1.7ml, the deionized water mix and blend 48h of the water glass solution of 5ml and 12.5ml, again mixing solutions is passed in strongly acidic styrene's resin of 25ml, after 10min, suction filtration obtains the silicon sol of pH=2.5, and the silicon sol with the 0.15g glass fibre after 120 ℃ of thermal treatment 24h adds above-mentioned suction filtration to obtain, stir 1h, add while stirring a certain amount of ammoniacal liquor, making the final pH value of system is 8.Stop after 10min stirring,, with the standing 24h of silicon dioxide gel, treat the sample gel.Gel is placed in ethanol solution carries out aging and solvent replacing, aging temperature is 50 ℃, after aging, gel sample is immersed in the solution batch volume than for TMCS: dehydrated alcohol: in the mixing solutions of normal hexane=2: 1: 8, modification is 2 days, wash away modification liquid with normal hexane, sample is immersed in normal hexane the drying that heats up under normal pressure, wherein, TMCS can adopt 5ml.
Drying process is: gel sample is incubated 6h under 45～50 ℃, speed with 1 ℃/min is warming up to 65 ℃, insulation 7h, speed with 1 ℃/min is warming up to 120 ℃ again, and insulation 5h, the speed with 1 ℃/min is warming up to 200 ℃ finally, insulation 6h, be chilled to room temperature with stove, namely obtain fibre-reinforced silicon dioxide composite aerogel.
The density that the glass fibre of described preparation strengthens silicon dioxide composite aerogel is 0.132g/cm
3, specific surface area is 625.2m
2/ g, mean pore size is 9.9nm, pore volume is 3.1cm
3/ g, hydrophobic angle is 147 °.
Embodiment 2
Material molar ratio is: water glass: MTMS: water=1: 0.2: 38, MTMS with 1.2ml, the deionized water mix and blend 24h of the water glass solution of 5ml and 13.5ml, again mixing solutions is passed in strongly acidic styrene's resin of 25ml, after 10min, suction filtration obtains the silicon sol of pH=2, and the silicon sol with the 0.2g glass fibre after 200 ℃ of thermal treatment 24h adds above-mentioned suction filtration to obtain, stir 1h, add while stirring a certain amount of ammoniacal liquor, making the final pH value of system is 8.1～8.2.Stop after 10min stirring,, with the standing 24h of silicon dioxide gel, treat the sample gel.Gel is placed in ethanol solution carries out aging and solvent replacing, aging temperature is 30 ℃, after aging, gel sample is immersed in the solution batch volume than for TMCS: dehydrated alcohol: in the mixing solutions of normal hexane=1: 3: 6, modification is 2 days, wash away modification liquid with normal hexane, sample is immersed in normal hexane the drying that heats up under normal pressure, wherein, TMCS can adopt 5ml.
Drying process is with embodiment 1.
The density that the glass fibre of described preparation strengthens silicon dioxide composite aerogel is 0.145g/cm
3, specific surface area is 706m
2/ g, mean pore size is 12nm, pore volume is 2.9cm
3/ g, hydrophobic angle is 148 °.
Embodiment 3
Material molar ratio is: water glass: MTES: water=1: 0.2: 40, MTES with 1.2ml, the deionized water mix and blend 24h of the water glass solution of 5ml and 14.3ml, remix solution passes in strongly acidic styrene's resin of 25ml, after 10min, suction filtration obtains the silicon sol of pH=2.5, and the silicon sol with the 0.15g glass fibre after 120 ℃ of thermal treatment 12h adds above-mentioned suction filtration to obtain, stir 30min, add while stirring a certain amount of ammoniacal liquor, make the final pH value of system 8.2～8.3.Stop after 10min stirring,, with the standing 24h of silicon dioxide gel, treat the sample gel.Gel is placed in ethanol solution carries out aging and solvent replacing, aging temperature is 30 ℃, after aging, gel sample is immersed in the solution batch volume than for TMCS: dehydrated alcohol: in the mixing solutions of normal hexane=1: 1: 8, modification is 2 days, wash away modification liquid with normal hexane, sample is immersed in normal hexane the drying that heats up under normal pressure, wherein, TMCS can adopt 5ml.
Drying process is with embodiment 1.
Embodiment 4
Material molar ratio is: water glass: MTES: water=1: 0.6: 30, MTES with 3.4ml, the deionized water mix and blend 24h of the water glass solution of 5ml and 10ml, remix solution passes in strongly acidic styrene's resin of 25ml, after 10min, suction filtration obtains the silicon sol of pH=3, and the silicon sol with the 0.1g glass fibre after 120 ℃ of thermal treatment 24h adds above-mentioned suction filtration to obtain, stir 30min, add while stirring a certain amount of ammoniacal liquor, make the final pH value of system 8.4～8.5.Stop after 10min stirring,, with the standing 24h of silicon dioxide gel, treat the sample gel.Gel is placed in ethanol solution carries out aging and solvent replacing, aging temperature is 30 ℃, after aging, gel sample is immersed in the solution batch volume than for TMCS: dehydrated alcohol: in the mixing solutions of normal hexane=1: 3: 6, modification is 2 days, wash away modification liquid with normal hexane, sample is immersed in normal hexane the drying that heats up under normal pressure.
Drying process is with embodiment 1.
Embodiment 5
Compare with embodiment 1, only change 120 ℃ of glass fibre after thermal treatment 24h and add quality in silicon sol, the quality that adds is 0.05g, and all the other preparation technologies are identical with embodiment 1.
The density of the glass fibre dioxide composite silica aerogel of described preparation is 0.143g/cm
3
Embodiment 6
Compare with embodiment 1, only change the modification in the mixing solutions that gel sample is immersed in TMCS, dehydrated alcohol and normal hexane, the add-on of TMCS is 8ml, and all the other preparation technologies are identical with embodiment 1.
The hydrophobic angle that the glass fibre of described preparation strengthens silicon dioxide composite aerogel is 152.6 °.
Embodiment 7
Compare with embodiment 2, only change the add-on of water glass in raw material, the add-on of water glass is 5.4ml, and all the other preparation technologies are identical with embodiment 2.
The density that the glass fibre of described preparation strengthens silicon dioxide composite aerogel is 0.105g/cm
3
Claims (10)
1. glass fibre strengthens the preparation method of water glass base silicon dioxide composite aerogel, it is characterized in that comprising the following steps:
1) the methyl TMOS mixed and stirs with water glass solution and deionized water, the methyl TMOS is hydrolyzed in deionized water, obtaining solution A;
2) solution A of step 1) preparation is added strongly acidic styrene's resin, carry out again ion-exchange, then suction filtration obtains the solution of pH=2～3, the solution that adds suction filtration to obtain in the glass fibre after thermal treatment, adding ammoniacal liquor regulation system pH value is 8～8.5 again, obtain the silicon dioxide gel of fiber composite, then transfer in container standingly, namely make compound silica hydrogel;
3) with step 2) the compound silica hydrogel that obtains is immersed in ethanol solution and carries out the aging of gel and alcoholization, after refining, the wet gel of gained is immersed in the mixing solutions of trimethylchlorosilane, dehydrated alcohol and normal hexane again, carry out surface modification, gel drying after modification, obtain glass fibre and strengthen water glass base silicon dioxide composite aerogel, prepared glass fibre strengthens water glass base silicon dioxide composite aerogel and is transparent block shape.
2. glass fibre strengthens the preparation method of water glass base silicon dioxide composite aerogel as claimed in claim 1, it is characterized in that in step 1), and described methyl TMOS adopts Union carbide A-162 or methyltrimethoxy silane.
3. glass fibre strengthens the preparation method of water glass base silicon dioxide composite aerogel as claimed in claim 1, it is characterized in that in step 1), press material molar ratio, described water glass solution: the methyl TMOS: deionized water is (0.8～1.2): (0.2～0.6): (30～40).
4. glass fibre strengthens the preparation method of water glass base silicon dioxide composite aerogel as claimed in claim 1, it is characterized in that in step 1), and the time of described stirring is 24～48h.
5. glass fibre strengthens the preparation method of water glass base silicon dioxide composite aerogel as claimed in claim 1, it is characterized in that in step 2) in, by volume, the solution A of step 1) preparation: strongly acidic styrene's resin is 0.5～2: 1.
6. glass fibre strengthens the preparation method of water glass base silicon dioxide composite aerogel as claimed in claim 1, it is characterized in that in step 2) in, describedly carry out standing 5～20min before ion-exchange; Described heat treated temperature is 120～200 ℃, and the heat treated time is 12～24h; It is described that to transfer to the time standing in container be 10～30min.
7. glass fibre strengthens the preparation method of water glass base silicon dioxide composite aerogel as claimed in claim 1, it is characterized in that in step 3), and by volume, described ethanol solution: compound silica hydrogel is (1.2～2): 1.
8. glass fibre strengthens the preparation method of water glass base silicon dioxide composite aerogel as claimed in claim 1, it is characterized in that in step 3), and described aging and temperature alcoholization is 25～60 ℃, and the time aging and alcoholization is 24～48h.
9. glass fibre strengthens the preparation method of water glass base silicon dioxide composite aerogel as claimed in claim 1, it is characterized in that in step 3), after described will the alcoholization, the wet gel of gained is immersed in the mixing solutions of trimethylchlorosilane, dehydrated alcohol and normal hexane, is to soak under air-proof condition 1～2 day; By volume, trimethylchlorosilane: dehydrated alcohol: normal hexane is (1～3): (1～3): (6～8).
10. glass fibre strengthens the preparation method of water glass base silicon dioxide composite aerogel as claimed in claim 1, it is characterized in that in step 3), the technical process of described drying is: the gel after modification, at 45～50 ℃ of insulation 6～8h, is warming up to 65～70 ℃, then is incubated 6～8h, and then be warming up to 120 ℃, be incubated again 4～6h, be warming up to finally 200 ℃, then be incubated 4～8h, stove is chilled to room temperature subsequently, and whole drying process heat-up rate is 1～5 ℃/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103431194A CN103396086A (en) | 2013-08-08 | 2013-08-08 | Preparation method for glass fiber-reinforced water glass-based silica composite aerogel |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103431194A CN103396086A (en) | 2013-08-08 | 2013-08-08 | Preparation method for glass fiber-reinforced water glass-based silica composite aerogel |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103396086A true CN103396086A (en) | 2013-11-20 |
Family
ID=49559879
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013103431194A Pending CN103396086A (en) | 2013-08-08 | 2013-08-08 | Preparation method for glass fiber-reinforced water glass-based silica composite aerogel |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103396086A (en) |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478395A (en) * | 2014-11-14 | 2015-04-01 | 刘吉海 | Composite SiO2 aerogel heat insulation material and preparation method thereof |
| CN105110339A (en) * | 2015-06-23 | 2015-12-02 | 北京建工新型建材有限责任公司 | Preparation method for low-cost flexible silica aerogel |
| CN105110340A (en) * | 2015-06-23 | 2015-12-02 | 北京建工新型建材有限责任公司 | Preparation method for elastic transparent silica aerogel |
| CN105418052A (en) * | 2015-11-09 | 2016-03-23 | 大连理工大学 | Preparation technology of carbon nanofiber composite silicon dioxide aerogel |
| CN105645921A (en) * | 2016-03-10 | 2016-06-08 | 深圳中凝科技有限公司 | Method for preparing composite SiO2 aerogel felt |
| CN105753439A (en) * | 2016-01-29 | 2016-07-13 | 卓达新材料科技集团有限公司 | Fiber punched felt/sliicon-alumininm aerogel composite insulation board |
| CN105776967A (en) * | 2016-01-29 | 2016-07-20 | 卓达新材料科技集团有限公司 | Preparation method for fiber needled felt-enhanced sodium metaaluminate-modified aerogel |
| CN106431186A (en) * | 2016-09-05 | 2017-02-22 | 北京工业大学 | Method for preparing fiber-loaded rutile type TiO2 composite SiO2 aerogel |
| CN106699216A (en) * | 2016-12-29 | 2017-05-24 | 北京华夏特材科技发展有限公司 | Preparation method of non-shedding elastic-aerogel-coated long fiber composite material |
| CN108101500A (en) * | 2017-12-06 | 2018-06-01 | 吕莉 | A kind of preparation method of high intensity spider silk dioxide composite silica aerogel |
| CN108395197A (en) * | 2018-03-19 | 2018-08-14 | 河南城建学院 | A kind of wall heat insulation material of the compound desulfurated plaster whisker of aerosil |
| CN109265131A (en) * | 2018-11-12 | 2019-01-25 | 中研信源（北京）节能科技有限公司 | A kind of preparation method of aerogel vacuum thermal insulation plate and its core material |
| CN109574621A (en) * | 2018-12-07 | 2019-04-05 | 上海交通大学 | Waterglass base fiber reinforcement type SiO2The fast preparation method of aerogel block body |
| CN110127706A (en) * | 2019-06-06 | 2019-08-16 | 广东工业大学 | A kind of preparation method of compound aerosil |
| CN113135732A (en) * | 2020-01-17 | 2021-07-20 | 北京蓝星清洗有限公司 | Chopped glass fiber silicon dioxide aerogel composite material and preparation method thereof |
| CN113564917A (en) * | 2020-04-29 | 2021-10-29 | 台湾气凝胶科技材料开发股份有限公司 | Preparation method and application of hydrophobic aerogel heat insulation material |
| CN114538891A (en) * | 2022-03-07 | 2022-05-27 | 东莞市零度导热材料有限公司 | One-step in-situ synthesis fiber-reinforced silica aerogel-based composite phase-change thermal insulation material and preparation method thereof |
| CN114835128A (en) * | 2022-05-31 | 2022-08-02 | 贵州航天乌江机电设备有限责任公司 | Preparation method of epoxy resin grafted modified silicon dioxide aerogel |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973752A (en) * | 2010-10-21 | 2011-02-16 | 厦门大学 | Glass fiber reinforced silicon dioxide aerogel composite material and preparation method thereof |
| CN102897779A (en) * | 2012-11-06 | 2013-01-30 | 厦门大学 | Preparation method of transparent silicon dioxide aerogel |
-
2013
- 2013-08-08 CN CN2013103431194A patent/CN103396086A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101973752A (en) * | 2010-10-21 | 2011-02-16 | 厦门大学 | Glass fiber reinforced silicon dioxide aerogel composite material and preparation method thereof |
| CN102897779A (en) * | 2012-11-06 | 2013-01-30 | 厦门大学 | Preparation method of transparent silicon dioxide aerogel |
Cited By (24)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104478395A (en) * | 2014-11-14 | 2015-04-01 | 刘吉海 | Composite SiO2 aerogel heat insulation material and preparation method thereof |
| CN105110339A (en) * | 2015-06-23 | 2015-12-02 | 北京建工新型建材有限责任公司 | Preparation method for low-cost flexible silica aerogel |
| CN105110340A (en) * | 2015-06-23 | 2015-12-02 | 北京建工新型建材有限责任公司 | Preparation method for elastic transparent silica aerogel |
| CN105110340B (en) * | 2015-06-23 | 2019-03-26 | 北京建工新型建材有限责任公司 | A kind of preparation method of elasticity transparent silicon dioxide aerogel |
| CN105418052A (en) * | 2015-11-09 | 2016-03-23 | 大连理工大学 | Preparation technology of carbon nanofiber composite silicon dioxide aerogel |
| CN105418052B (en) * | 2015-11-09 | 2018-08-28 | 大连理工大学 | A kind of preparation process of carbon nano-fiber combined oxidation silica aerogel |
| CN105776967A (en) * | 2016-01-29 | 2016-07-20 | 卓达新材料科技集团有限公司 | Preparation method for fiber needled felt-enhanced sodium metaaluminate-modified aerogel |
| CN105753439A (en) * | 2016-01-29 | 2016-07-13 | 卓达新材料科技集团有限公司 | Fiber punched felt/sliicon-alumininm aerogel composite insulation board |
| CN105645921A (en) * | 2016-03-10 | 2016-06-08 | 深圳中凝科技有限公司 | Method for preparing composite SiO2 aerogel felt |
| CN105645921B (en) * | 2016-03-10 | 2018-03-06 | 深圳中凝科技有限公司 | One kind prepares composite S iO2The method of aerogel blanket |
| CN106431186A (en) * | 2016-09-05 | 2017-02-22 | 北京工业大学 | Method for preparing fiber-loaded rutile type TiO2 composite SiO2 aerogel |
| CN106431186B (en) * | 2016-09-05 | 2019-03-29 | 北京工业大学 | A kind of fiber-loaded rutile TiO2Composite S iO2The preparation method of aeroge |
| CN106699216A (en) * | 2016-12-29 | 2017-05-24 | 北京华夏特材科技发展有限公司 | Preparation method of non-shedding elastic-aerogel-coated long fiber composite material |
| CN108101500A (en) * | 2017-12-06 | 2018-06-01 | 吕莉 | A kind of preparation method of high intensity spider silk dioxide composite silica aerogel |
| CN108395197A (en) * | 2018-03-19 | 2018-08-14 | 河南城建学院 | A kind of wall heat insulation material of the compound desulfurated plaster whisker of aerosil |
| CN109265131A (en) * | 2018-11-12 | 2019-01-25 | 中研信源（北京）节能科技有限公司 | A kind of preparation method of aerogel vacuum thermal insulation plate and its core material |
| CN109265131B (en) * | 2018-11-12 | 2021-06-15 | 王贵然 | Aerogel vacuum insulation panel and preparation method of core material thereof |
| CN109574621A (en) * | 2018-12-07 | 2019-04-05 | 上海交通大学 | Waterglass base fiber reinforcement type SiO2The fast preparation method of aerogel block body |
| CN109574621B (en) * | 2018-12-07 | 2020-09-15 | 上海交通大学 | Water glass-based fiber reinforced SiO2Rapid preparation method of aerogel block |
| CN110127706A (en) * | 2019-06-06 | 2019-08-16 | 广东工业大学 | A kind of preparation method of compound aerosil |
| CN113135732A (en) * | 2020-01-17 | 2021-07-20 | 北京蓝星清洗有限公司 | Chopped glass fiber silicon dioxide aerogel composite material and preparation method thereof |
| CN113564917A (en) * | 2020-04-29 | 2021-10-29 | 台湾气凝胶科技材料开发股份有限公司 | Preparation method and application of hydrophobic aerogel heat insulation material |
| CN114538891A (en) * | 2022-03-07 | 2022-05-27 | 东莞市零度导热材料有限公司 | One-step in-situ synthesis fiber-reinforced silica aerogel-based composite phase-change thermal insulation material and preparation method thereof |
| CN114835128A (en) * | 2022-05-31 | 2022-08-02 | 贵州航天乌江机电设备有限责任公司 | Preparation method of epoxy resin grafted modified silicon dioxide aerogel |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103396086A (en) | Preparation method for glass fiber-reinforced water glass-based silica composite aerogel | |
| CN101973752B (en) | Glass fiber reinforced silicon dioxide aerogel composite material and preparation method thereof | |
| CN102351494B (en) | Method for preparing foam material reinforced silica aerogel composite material | |
| CN102897779B (en) | Preparation method of transparent silicon dioxide aerogel | |
| CN108467276A (en) | A kind of preparation method of electrostatic spinning nano fiber enhancing aerosil | |
| CN107140938B (en) | A kind of anti-shedding aeroge complex heat-preservation felt and preparation method thereof | |
| CN103708476B (en) | A kind of preparation method of flexible silica aerogel | |
| CN104478394B (en) | A kind of fiber felt strengthens the preparation method of aerosil composite plate | |
| CN106629750B (en) | A kind of atmospheric preparation method of transparent silicon dioxide block aeroge | |
| CN101372337B (en) | Method for preparing transparent silicon dioxide aerogel by co-precursor normal atmosphere drying | |
| CN102557577B (en) | Preparation method of silicon dioxide aerogel composite material | |
| CN106747262B (en) | A kind of preparation method of the super composite heat-insulated material of nano grade silica particles base | |
| CN103011745A (en) | Silicon-dioxide aerogel heat insulation composite material and preparation method thereof | |
| CN111607253B (en) | Preparation method of silica aerogel thermal insulation filler | |
| CN103922643B (en) | Composite SiO2 aerogel heat-insulation felt pad and preparation method | |
| CN101254449A (en) | Preparation of oxide nano thread reinforced transparency aerogel block body material | |
| CN103203206A (en) | Cellulose/titanium dioxide/silica aerogel and preparation method thereof | |
| CN107263948B (en) | A kind of fire-proof thermal-insulation decoration and preparation method thereof | |
| CN101633505A (en) | SiO2 nanoscale porous material with aerogel property prepared by microwave reaction and preparation method thereof | |
| WO2014110892A1 (en) | Inorganic thermal insulation material and preparation method thereof | |
| CN105198375A (en) | Thermal insulation silicon dioxide aerogel/hydroxylation glass fiber felt composite and preparation method thereof | |
| CN104071797A (en) | Method for preparing silicon dioxide aerogel coating with low density and large specific surface area by water glass at normal pressure and room temperature | |
| CN104496401B (en) | Effectively insulating Aerogel composite board material and preparation method thereof | |
| CN109851380A (en) | A kind of preparation method of aerosil functional material | |
| CN109701494B (en) | Aerogel composite material and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20131120 |