CN107504326A - A kind of SiO2Aerogel microball vacuum heat-insulating plate and preparation method thereof - Google Patents
A kind of SiO2Aerogel microball vacuum heat-insulating plate and preparation method thereof Download PDFInfo
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- CN107504326A CN107504326A CN201710657787.2A CN201710657787A CN107504326A CN 107504326 A CN107504326 A CN 107504326A CN 201710657787 A CN201710657787 A CN 201710657787A CN 107504326 A CN107504326 A CN 107504326A
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L59/00—Thermal insulation in general
- F16L59/02—Shape or form of insulating materials, with or without coverings integral with the insulating materials
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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Abstract
The invention discloses a kind of SiO2Aerogel microball vacuum heat-insulating plate and preparation method thereof, belong to insulation and heat-barrier material field, the SiO2Aerogel microball vacuum heat-insulating plate is by SiO2Aerogel microball core, getter, barrier film composition；Microspheroidal SiO is prepared using sol gel process2Alcogel, replaced by colloidal sol, surface modification, constant pressure and dry, the technique such as screening prepare SiO2Aerogel microball, then by SiO2Aerogel microball and getter enclose barrier film, by vacuumizing obtained SiO2Aerogel microball vacuum heat-insulating plate.The present invention preparation technology have easily vacuumize, be easily-controllable, low power consumption and other advantages, the aerogel microball vacuum heat-insulating plate of preparation has the characteristics that ultralight, pressure-bearing is good, superthermal insulation, low vacuum, hydrophobic, having the advantages that vacuum to hold time in engineer applied, long, service life is long, in fields such as building, industry, Refrigerated Transports with extensive use space.
Description
Technical field
The present invention relates to heat-barrier material technical field, more particularly to a kind of SiO2Aerogel microball vacuum heat-insulating plate and its system
Preparation Method.
Background technology
With the continuous increase to the demand of the energy of fast development and the mankind of social economy, improve energy utilization rate with
Realize that energy-conserving and environment-protective turn into study hotspot both domestic and external.To 2013, Energy Consumption of Public Buildings accounted for the 24.8% of building total energy consumption,
Wherein 95% above is high energy consumption is built, and building energy consumption is into an important factor for restriction Chinese society economic development.By reasonable
Good energy-saving effect can be obtained from energy-efficient construction material, the application of heat preserving and insulating material is to realize that building energy consumption drops
Low effective way.
SiO2Aeroge is current density minimum (as little as 0.003gcm-3) and heat-proof quality is preferably (under normal temperature as little as
0.013W·m-1·K-1) Performances of Novel Nano-Porous metre hole multifunctional solid material, have in fields such as physics, calorifics, optics and electricity wide
General development and application prospect.Aeroge has contact angle up to 160 ° of super-hydrophobicity after being handled by special process, simultaneously
Also there is the characteristics such as corrosion-resistant, high temperature resistant, be a kind of excellent heat-insulating heat-preserving material.Conventional heat preserving and insulating material is main at present
There are EPS foamed polystyrene boards, PIR PICs, PU polyurethane, rock cotton board etc..
Recently using aerosil powder etc. as core, the vacuum heat-insulating plate prepared by vacuum technology etc., with
Common porous material is compared, due to having more preferable heat-insulating property it significantly reduces gas phase heat conduction.But with gas phase titanium dioxide
The vacuum heat-insulating plate as core such as silicon powder, vacuumizing preparation process should not control, and vacuum heat-insulating plate load performance is poor, vacuum
Degree hold time it is short, make its service life life-span shorter, limit the development and application of vacuum heat-insulating plate.
The content of the invention
It is an object of the invention to provide a kind of SiO2Aerogel microball vacuum heat-insulating plate and preparation method thereof, the aeroge
Microballoon vacuum heat-insulating plate is by SiO2Aerogel microball core, getter, barrier film composition, it is obtained by vacuumizing, sealing.The present invention
With microspheroidal SiO2Aeroge has ultra-low thermal conductivity for the vacuum heat-insulating plate of core, easily vacuumized, the spy such as load performance is good
Point, having the advantages that vacuum to hold time in engineer applied, long, service life is long, in the neck such as building, industry, Refrigerated Transport
Domain has extensively using space.
In order to achieve the above object, the present invention adopts the following technical scheme that：
A kind of SiO2Aerogel microball vacuum heat-insulating plate, including Obstruct membrane, vacuum seal is equipped with SiO in Obstruct membrane2Aeroge is micro-
Ball and getter, are made SiO2Aerogel microball vacuum heat-insulating plate,
The SiO2Aerogel microball surface is hydrophobicity, and its particle diameter is 1~100 μm, and porosity is 80~99%, hole
Diameter is 10~50nm.
Further, the SiO2Aerogel microball and getter weight ratio are 102:1~104:1。
Further, the getter is can to absorb N2、O2、CO2、H2It is barium-lithium alloy, oxygen with the material of water vapour
Change one kind or two or more in cobalt, activated carbon, barium monoxide and calcium oxide.
Further, the Obstruct membrane is that have trapping, heat-insulated and some strength characteristic material, is metal film, aluminium-poly-
Any one in ester composite membrane glass (AF) or multilayer aluminized polyester film (MF).
A kind of SiO2The preparation method of aerogel microball vacuum heat-insulating plate, step are as follows：
(1) SiO2Aerogel microball is sieved, and obtains the SiO that particle size range is 1~100 μm2Aerogel microball；
(2) with SiO2Aerogel microball is core, is proportionally added into getter mixing；
(3) mixing material of step (2) is put into barrier film, is sealed using vacuum packing machine, SiO is made2Airsetting
Glue microballoon vacuum heat-insulating plate.
Further, the pressure that sealing terminates in rear heat-insulating shield is 10-1~104Pa。
A kind of SiO2The preparation method of aerogel microball, comprises the following steps：
(1) Ludox pH value is adjusted to 1~2 for 1~10% hydrochloric acid with mass concentration at room temperature；
(2) under conditions of stirring, the water of the addition volume of Ludox 0.1~3 and the absolute ethyl alcohol of 1~10 volume are dilute
Ludox is released, is stood after stirring 10min；
(3) normal heptane, Span 80, polysorbate85, n-butanol are measured oil phase liquid is made, Ludox is added in oil phase liquid, made
It forms uniform water-in-oil emulsion；
(4) pH value of emulsion is adjusted to 7~10, is dispersed in oil toward concentrated ammonia liquor is added in water-in-oil emulsion while stirring
Colloidal sol fine particle gel precipitation in phase, separation of solid and liquid obtain microspheroidal SiO2Alcogel；
(5) ethanol cleaning microspheroidal SiO2Alcogel, remove the oil phase of residual；
(6) ageing and aging microspheroidal SiO2Alcogel；
(7) solvent is replaced；
(8) surface modification；
(9) microspheroidal SiO is cleaned2Alcogel；
(10) drying process, by the microspheroidal SiO after cleaning2Alcogel is placed in drying box and obtained using constant pressure and dry
SiO2Aerogel microball.
Further, the step (3), counts, normal heptane by volume：Span 80：Polysorbate85：N-butanol=1000：1~
10：0.1~1：25~100；
Low whipping speed is 500~1500rmin-1It is lower that Ludox is added in oil phase liquid, count, add by volume
Measure as oil/Ludox=2.5~10：1, form uniform water-in-oil emulsion.
Further, the step (4), the colloidal sol fine particle precipitation being dispersed in after ph value of emulsion rise in oil phase, this
When start mixing speed to be reduced to 500~700rmin-1, continue stirring 15~60 minutes, then separation of solid and liquid, obtain micro-
Spherical SiO2Alcogel.
Further, in the step (6), microspheroidal SiO is aged at room temperature2Alcogel, it is then to go with volume ratio
Ionized water：Ethanol=1:3~1:10 mixed liquor is tetraethyl orthosilicate to the primary aging of gel progress, then with volume ratio：Ethanol
=1:3~1:10 mother liquor carries out two level aging to gel；
In the step (7), the microspheroidal SiO that is finished with the small solution of surface tension to aging2Alcogel carries out solvent
Displacement；
In the step (8), using hydrophobic agents and the small solution of surface tension by volume 1:100~3:10 mixing,
Microspheroidal SiO2 alcogel is soaked in the mixed liquor；
In the step (9), the microspheroidal SiO that is finished using the small solution of surface tension to surface modification2Alcogel enters
Row surface clean, remove the modified outcome of its remained on surface；
The small solution of surface tension is the one or more in n-hexane, normal heptane, acetone in step (7)~(9).
Step (8) hydrophobic agents be trim,ethylchlorosilane, HMDS, dimethyldimethoxysil,ne,
One or more in ethyl dibutyl silane.
The advantage of the invention is that：
1) present invention uses core of the SiO2 aerogel microballs as vacuum heat-insulating plate, compared to existing gas phase titanium dioxide
The cores such as silicon, glass fibre have the advantages that density is small, porosity is high, aperture size is small, make SiO2Aerogel microball vacuum is exhausted
Hot plate thermal conductivity factor is smaller, and with preferably insulation and heat-proof quality；
2) SiO prepared by the present invention2The inside core of aerogel microball vacuum heat-insulating plate has good hydrophobicity, improves
The moisture resistivity and service life of vacuum heat-insulating plate；
3) SiO of the present invention2Aerogel microball core has good support and the Stability Analysis of Structures such as pressure-resistant to vacuum heat-insulating plate
Property, make the preparation technology that vacuumizes of vacuum heat-insulating plate there are easily-controllable, low power consumption and other advantages, and make SiO2Aerogel microball vacuum
Heat-insulating shield is not easy to be damaged in insulation application process, has the advantages that stability, service life are long.
Brief description of the drawings
Accompanying drawing described herein is used for providing a further understanding of the present invention, forms the part of the application, not
Inappropriate limitation of the present invention is formed, in the accompanying drawings：
Fig. 1 is SiO2The structural map of aerogel microball vacuum heat-insulating plate.
Embodiment
The present invention is described in detail below in conjunction with accompanying drawing and specific embodiment, herein with the schematic implementation of the present invention
Example and explanation are used for explaining the present invention, but not as a limitation of the invention.
Embodiment one
Prepare SiO2Aerogel microball, comprise the following steps that：
(1) at room temperature, measure mass content be 25% Ludox 20mL, with mass concentration be 10% hydrochloric acid Ludox
PH value is adjusted to 2；
(2) dilution is stirred with 4mL deionized water and 40mL absolute ethyl alcohols, stands 12h；
(3) by volume, normal heptane is measured：Span 80：Polysorbate85：N-butanol=800：1：0.15：25, it is configured to oil
Phase.Low whipping speed is 1000rmin-1It is lower that the Ludox previously prepared is added dropwise in oil phase liquid, by volume, add
It is oil phase/Ludox 5 to enter amount：1, form it into uniform water-in-oil emulsion；
(4) under stirring, concentrated ammonia liquor is added, the pH value of whole emulsion is increased to 8, the colloidal sol being dispersed in oil phase
Fine particle, due to the rise of pH value, gel precipitation gets off quickly, and reduction mixing speed is 600rmin-1, 30min is stirred for,
Stop stirring, separation of solid and liquid, obtain microspheroidal SiO2Alcogel；
(5) microspheroidal SiO is cleaned with ethanol2Alcogel, remove the oil phase of residual；
(6) microspheroidal SiO is aged at room temperature2Alcogel, it is deionized water with volume ratio：Ethanol=1:5 mixed liquor
It is tetraethyl orthosilicate to the primary aging of gel progress, then with volume ratio：Ethanol=1:5 mother liquor carries out two level aging to gel；
(7) the microspheroidal SiO finished with the small n-hexane of surface tension to aging2Alcogel carries out solvent displacement；
(8) using trim,ethylchlorosilane and n-hexane by volume 1:50 mixing, by microspheroidal SiO2Alcogel is mixed at this
Close and soaked in liquid.
(9) the microspheroidal SiO finished using n-hexane to surface modification2Alcogel carries out surface clean, and it is residual to remove surface
The modified outcome stayed.
(10) gel through over cleaning is placed in progress constant pressure and dry in drying box and obtains SiO2Aerogel microball.
A kind of SiO2Aerogel microball vacuum heat-insulating plate, including Obstruct membrane, vacuum seal is equipped with SiO in Obstruct membrane2Aeroge is micro-
Ball and getter, are made SiO2Aerogel microball vacuum heat-insulating plate,
The SiO2Aerogel microball surface is hydrophobicity, and its particle diameter is 20~70 μm, and porosity is 93%, pore diameter
It is 15~40nm.
The SiO2Aerogel microball and getter weight ratio are 1000:1.
A kind of preparation method of aerogel microball vacuum heat-insulating plate, step are as follows：
(1) SiO2Aerogel microball is sieved, and obtains the SiO that particle size range is 20~70 μm2Aerogel microball；
(2) with the SiO of screening2Aerogel microball is core, using Combo getter SAES as getter, with aluminium-polyester
High impedance barrier film (PET12/Al7/CPP70) it is Obstruct membrane, by the SiO of screening2Aerogel microball is inhaled with Combo getter SAES
Gas agent mixes；
(3) mixing material of step (2) is put into barrier film, after putting Obstruct membrane into, sealed using vacuum packing machine,
SiO is made2Aerogel microball vacuum heat-insulating plate, the vacuum that sealing terminates rear heat-insulating shield is 1Pa.
Embodiment two
Prepare SiO2Aerogel microball, comprise the following steps that：
(1) at room temperature, measure mass content be 25% Ludox 20mL, with mass concentration be 10% hydrochloric acid Ludox
PH value is adjusted to 2；
(2) dilution is stirred with 10mL deionized water and 30mL absolute ethyl alcohols, stands 12h；
(3) by volume, normal heptane is measured：Span 80：Polysorbate85：N-butanol=1000：3：0.5：60, it is configured to oil
Phase, low whipping speed 500rmin-1It is lower that the Ludox previously prepared is added dropwise in oil phase liquid, by volume, add
Measure as oil phase/Ludox 2.5：1, form it into uniform water-in-oil emulsion；
(4) under stirring, concentrated ammonia liquor is added, the pH value of whole emulsion is increased to 7, the colloidal sol being dispersed in oil phase
Fine particle, due to the rise of pH value, gel precipitation gets off quickly, and reduction mixing speed is 500rmin-1, 60min is stirred for,
Stop stirring, separation of solid and liquid, obtain microspheroidal SiO2Alcogel；
(5) microspheroidal SiO is cleaned with ethanol2Alcogel, remove the oil phase of residual；
(6) microspheroidal SiO is aged at room temperature2Alcogel, it is deionized water with volume ratio：Ethanol=1:4 mixed liquor
It is tetraethyl orthosilicate to the primary aging of gel progress, then with volume ratio：Ethanol=1:4 mother liquor carries out two level aging to gel；
(7) the microspheroidal SiO finished with the small n-hexane of surface tension to aging2Alcogel carries out solvent displacement；
(8) using trim,ethylchlorosilane and n-hexane by volume 1:100 mixing, by microspheroidal SiO2Alcogel is mixed at this
Close and soaked in liquid.
(9) the microspheroidal SiO finished using n-hexane to surface modification2Alcogel carries out surface clean, and it is residual to remove surface
The modified outcome stayed.
(10) gel through over cleaning is placed in progress constant pressure and dry in drying box and obtains SiO2Aerogel microball.
A kind of SiO2Aerogel microball vacuum heat-insulating plate, including Obstruct membrane, vacuum seal is equipped with SiO in Obstruct membrane2Aeroge is micro-
Ball and getter, are made SiO2Aerogel microball vacuum heat-insulating plate,
The SiO2Aerogel microball surface is hydrophobicity, and its particle diameter is 10~80 μm, and porosity is 87%, pore diameter
It is 10~35nm..
The SiO2Aerogel microball and getter weight ratio are 500:1.
A kind of preparation method of aerogel microball vacuum heat-insulating plate, step are as follows：
(1) SiO2Aerogel microball is sieved, and obtains the SiO that particle size range is 10~80 μm2Aerogel microball；
(2) with the SiO of screening2Aerogel microball is core, using Combo getter SAES as getter, with aluminium-polyester
High impedance barrier film (PET12/Al7/CPP70) it is Obstruct membrane, by the SiO of screening2Aerogel microball is inhaled with Combo getter SAES
Gas agent mixes；
(3) mixing material of step (2) is put into barrier film, after putting Obstruct membrane into, sealed using vacuum packing machine,
SiO is made2Aerogel microball vacuum heat-insulating plate, the vacuum that sealing terminates rear heat-insulating shield is 10Pa.
Embodiment three
Prepare SiO2Aerogel microball, comprise the following steps that：
(1) at room temperature, measure mass content be 25% Ludox 20mL, with mass concentration be 10% hydrochloric acid Ludox
PH value is adjusted to 2；
(2) dilution is stirred with 60mL deionized water and 100mL absolute ethyl alcohols, stands 12h；
(3) by volume, normal heptane is measured：Span 80：Polysorbate85：N-butanol=1000：10：1：100, it is configured to oil
Phase.Low whipping speed is 1500rmin-1It is lower that the Ludox previously prepared is added dropwise in oil phase liquid, by volume, add
It is oil phase/Ludox 10 to enter amount：1, form it into uniform water-in-oil emulsion；
(4) under stirring, concentrated ammonia liquor is added, the pH value of whole emulsion is increased to 8, the colloidal sol being dispersed in oil phase
Fine particle, due to the rise of pH value, gel precipitation gets off quickly, and reduction mixing speed is 700rmin-1, 30min is stirred for,
Stop stirring, separation of solid and liquid, obtain microspheroidal SiO2Alcogel；
(5) microspheroidal SiO is cleaned with ethanol2Alcogel, remove the oil phase of residual；
(6) microspheroidal SiO is aged at room temperature2Alcogel, it is deionized water with volume ratio：Ethanol=1:10 mixed liquor
It is tetraethyl orthosilicate to the primary aging of gel progress, then with volume ratio：Ethanol=1:10 mother liquor carries out two level aging to gel；
(7) the microspheroidal SiO finished with the small n-hexane of surface tension to aging2Alcogel carries out solvent displacement；
(8) using trim,ethylchlorosilane and n-hexane by volume 3：10 mixing, by microspheroidal SiO2Alcogel is mixed at this
Close and soaked in liquid.
(9) the microspheroidal SiO finished using n-hexane to surface modification2Alcogel carries out surface clean, and it is residual to remove surface
The modified outcome stayed.
(10) gel through over cleaning is placed in progress constant pressure and dry in drying box and obtains SiO2Aerogel microball.
A kind of SiO2Aerogel microball vacuum heat-insulating plate, including Obstruct membrane, vacuum seal is equipped with SiO in Obstruct membrane2Aeroge is micro-
Ball and getter, are made SiO2Aerogel microball vacuum heat-insulating plate,
The SiO2Aerogel microball surface is hydrophobicity, and its particle diameter is 30~90 μm, and porosity is 92%, pore diameter
It is 10~50nm..
The SiO2Aerogel microball and getter weight ratio are 800:1.
A kind of preparation method of aerogel microball vacuum heat-insulating plate, step are as follows：
(1) SiO2Aerogel microball is sieved, and obtains the SiO that particle size range is 30~90 μm2Aerogel microball；
(2) with the SiO of screening2Aerogel microball is core, using Combo getter SAES as getter, with aluminium-polyester
High impedance barrier film (PET12/Al7/CPP70) it is Obstruct membrane, by the SiO of screening2Aerogel microball is inhaled with Combo getter SAES
Gas agent mixes；
(3) mixing material of step (2) is put into barrier film, after putting Obstruct membrane into, sealed using vacuum packing machine,
SiO is made2Aerogel microball vacuum heat-insulating plate, it is 50Pa that sealing, which terminates pressure in rear heat-insulating shield,.
The experimental data of each embodiment such as table 1 below：
| Embodiment one | Embodiment two | Embodiment three | |
| Thermal conductivity factor | 1.6mW/m+K | 2.1mW/m+K | 3.9mW/m+K |
| Compressive strength | 0.24MPa | 0.38MPa | 0.51MPa |
The technical scheme provided above the embodiment of the present invention is described in detail, specific case used herein
The principle and embodiment of the embodiment of the present invention are set forth, the explanation of above example is only applicable to help and understands this
The principle of inventive embodiments；Meanwhile for those of ordinary skill in the art, according to the embodiment of the present invention, in specific embodiment party
There will be changes in formula and application, in summary, this specification content should not be construed as limiting the invention.
Claims (10)
- A kind of 1. SiO2Aerogel microball vacuum heat-insulating plate, it is characterised in that：Including Obstruct membrane, vacuum seal is equipped with SiO in Obstruct membrane2Aerogel microball and getter, are made SiO2Aerogel microball vacuum Heat-insulating shield,The SiO2Aerogel microball surface is hydrophobicity, and its particle diameter is 1~100 μm, and porosity is 80~99%, pore diameter It is 10~50nm.
- A kind of 2. SiO according to claim 12Aerogel microball vacuum heat-insulating plate, it is characterised in that：The SiO2Aeroge Microballoon and getter weight ratio are 102:1~104:1。
- A kind of 3. SiO according to claim 12Aerogel microball vacuum heat-insulating plate, it is characterised in that：The getter is energy Enough absorb N2、O2、CO2、H2It is 1 in barium-lithium alloy, cobalt oxide, activated carbon, barium monoxide and calcium oxide with the material of water vapour Kind or two or more.
- A kind of 4. SiO according to claim 12Aerogel microball vacuum heat-insulating plate, it is characterised in that：The Obstruct membrane is tool There are trapping, heat-insulated and some strength characteristic material, be metal film, aluminium-polyester compound film glass (AF) or multilayer aluminized polyester film (MF) any one in.
- A kind of 5. SiO as claimed in claim 12The preparation method of aerogel microball vacuum heat-insulating plate, it is characterised in that：Step is as follows：(1) SiO2Aerogel microball is sieved, and obtains the SiO that particle size range is 1~100 μm2Aerogel microball；(2) with SiO2Aerogel microball is core, is proportionally added into getter mixing；(3) mixing material of step (2) is put into barrier film, is sealed using vacuum packing machine, SiO is made2Aerogel microball Vacuum heat-insulating plate.
- A kind of 6. preparation method of aerogel microball vacuum heat-insulating plate according to claim 5, it is characterised in that：It is 10 to seal the pressure terminated in rear heat-insulating shield-1~104Pa。
- A kind of 7. SiO2The preparation method of aerogel microball, it is characterised in that：Comprise the following steps：(1) Ludox pH value is adjusted to 1~2 for 1~10% hydrochloric acid with mass concentration at room temperature；(2) under conditions of stirring, the water of the volume of Ludox 0.1~3 and the absolute ethyl alcohol dilution silicon of 1~10 volume are added Colloidal sol, stood after stirring 10min；(3) normal heptane, Span 80, polysorbate85, n-butanol are measured oil phase liquid is made, Ludox is added in oil phase liquid, makes its shape Into uniform water-in-oil emulsion；(4) pH value of emulsion is adjusted to 7~10, is dispersed in oil phase toward concentrated ammonia liquor is added in water-in-oil emulsion while stirring Colloidal sol fine particle gel precipitation, separation of solid and liquid obtains microspheroidal SiO2Alcogel；(5) ethanol cleaning microspheroidal SiO2Alcogel, remove the oil phase of residual；(6) ageing and aging microspheroidal SiO2Alcogel；(7) solvent is replaced；(8) surface modification；(9) microspheroidal SiO is cleaned2Alcogel；(10) drying process, by the microspheroidal SiO after cleaning2Alcogel is placed in drying box and obtains SiO using constant pressure and dry2Gas Gel micro-ball.
- A kind of 8. SiO according to claim 72The preparation method of aerogel microball, it is characterised in that：The step (3), counts, normal heptane by volume：Span 80：Polysorbate85：N-butanol=1000：1~10：0.1~1：25 ~100；Low whipping speed is 500~1500rmin-1It is lower that Ludox is added in oil phase liquid, count by volume, addition is Oil/Ludox=2.5~10：1, form uniform water-in-oil emulsion.
- A kind of 9. SiO according to claim 72The preparation method of aerogel microball, it is characterised in that：The step (4), the colloidal sol fine particle precipitation being dispersed in after ph value of emulsion rise in oil phase, now starts stirring speed Degree is reduced to 500~700rmin-1, continue stirring 15~60 minutes, then separation of solid and liquid, obtain microspheroidal SiO2Alcogel.
- A kind of 10. SiO according to claim 72The preparation method of aerogel microball, it is characterised in that：In the step (6), microspheroidal SiO is aged at room temperature2Alcogel, it is then deionized water with volume ratio：Ethanol=1: 3~1:10 mixed liquor is tetraethyl orthosilicate to the primary aging of gel progress, then with volume ratio：Ethanol=1:3~1:10 mother Liquid carries out two level aging to gel；In the step (7), the microspheroidal SiO that is finished with the small solution of surface tension to aging2Alcogel carries out solvent displacement；In the step (8), using hydrophobic agents and the small solution of surface tension by volume 1:100~3:10 mixing, will be micro- Spherical sio2 alcogel is soaked in the mixed liquor；In the step (9), the microspheroidal SiO that is finished using the small solution of surface tension to surface modification2Alcogel carries out surface Cleaning, remove the modified outcome of its remained on surface；The small solution of surface tension is the one or more in n-hexane, normal heptane, acetone in step (7)~(9)；Step (8) hydrophobic agents are trim,ethylchlorosilane, HMDS, dimethyldimethoxysil,ne, ethyl One or more in dibutyl silane.
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Cited By (1)
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