CN105198375B - Thermal insulation silicon dioxide aerogel/hydroxylation glass fiber felt composite and preparation method thereof - Google Patents
Thermal insulation silicon dioxide aerogel/hydroxylation glass fiber felt composite and preparation method thereof Download PDFInfo
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- CN105198375B CN105198375B CN201510601263.2A CN201510601263A CN105198375B CN 105198375 B CN105198375 B CN 105198375B CN 201510601263 A CN201510601263 A CN 201510601263A CN 105198375 B CN105198375 B CN 105198375B
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Abstract
The invention discloses a thermal insulation silicon dioxide aerogel/hydroxylation glass fiber felt composite and a preparation method thereof. The thermal insulation silicon dioxide aerogel/hydroxylation glass fiber felt composite is characterized in that silicon dioxide aerogel accounts for 50-80 weight parts of a matrix, and hydroxylation glass fiber felt accounts for 70-120 weight parts of a reinforcing body. The thermal insulation silicon dioxide aerogel/hydroxylation glass fiber felt composite is prepared by preparing a silica sol system of an MQ structure (M represents (CH3)3SiO1/2, Q represents SiO4/2) through raw materials including absolute ethyl alcohol, deionized water, hexamethyldisiloxane and the like under the acid catalysis environment, then adding gel catalysts, submerging preprocessed glass fiber in the silica sol system to form a wet gel and fiber felt composite, conducting soaking through normal hexane after ageing is conducted for 12-24 h so that water in the system can be removed, and conducting drying to obtain the silicon dioxide aerogel/hydroxylation glass fiber felt composite at temperature of 50-120 DEG C and pressure of 0.01-5 Pa for 1-5 h.
Description
Technical field
The present invention relates to a kind of adiabatic aerosil/hydroxylating glass fibre felt composite material and its preparation side
Method, belongs to aerogel composite preparing technical field.
Technical background
Aerosil is a kind of high-specific surface area, low-density and the ultralight porous material with three-dimensional manometer pore structure
Material, has unique optics, acoustics, electricity, calorifics premium properties, in Aeronautics and Astronautics, metallurgy, petrochemical industry and energy-saving building material
Field has a wide range of applications.
At present, preparation and application to aeroge of Chinese scholars and enterprise is conducted extensive research, using organosilicon
As silicon source, using-gel process is dissolved, after dried, you can form aerosil.But, because close
Spend extremely low (about the 1/6～1/3 of atmospheric density), specific surface area is high, and porosity is up to 99%, cause mechanical strength spy it is low,
Big Monolithic aerogel difficult forming, significantly limit the application of the material, therefore, it is necessary to increase to aerosil
The improvement of strong toughness reinforcing is to meet various forms of heat-insulated needs, and realizes aeroge commercial application.
Conventional drying process is mostly critical, or supercritical drying, and this technique is accompanied by high temperature and high pressure environment, in reactor
Middle long-time is dried process, carries out industrialized production, with certain danger, thus be devoted under this harsh conditions
Constant pressure and dry airsetting adhesive process, is beneficial to the industrialized production of aeroge.
Because of the special construction of itself, aeroge determines that intensity is extremely low, so as to be difficult to carry out each section bars such as big bulk, tabular
Production, according to the requirement of some special application fields, composited processing need to be carried out to aeroge, it is desirable to both ensureing aeroge
While performance, the overall mechanical strength of material, and the processing characteristics of composite are improved.
Chinese patent CN1592651A provides a kind of preparation method of aerogel heat-insulating composite material, prepared by the technique
Aerogel composite better performances, relative cost are higher, mainly using supercritical drying process, have in industrialized production
Certain danger, is unfavorable for industrialization large-scale production.
Chinese patent CN103342537A provides a kind of preparation method of high temperature-resistanalumina alumina aerogel material, this technique
The aeroge intensity of preparation is high, block big, shows the larger prospect of marketing, but since it is desired that supercritical equipment,
Simultaneously need through high temperature high pressure process, thus, for commercially producing also certain limitation.
Chinese patent CN102351506A provides a kind of preparation side of block high temperature resistant silicon-charcoal composite aerogel material
The shortcoming of method, aeroge resistance to elevated temperatures difference and intensity not easy-formation, the aeroge of preparation can be in 1000 DEG C of high temperature above
Long-time is used, with low-density, bigger serface, big pore volume, high intensity, high-temperature stability.The great advantage of the material is
Resistance to 1000 DEG C of high temperature, but the pliability and service life of its material are limited.It is unfavorable for large-scale production.
The content of the invention：
The purpose of the present invention is to provide a kind of adiabatic aerosil/glass mat for the deficiencies in the prior art
Composite and preparation method thereof, is characterized in based on aerosil, and intensity is up to 132KPa, and density is 200
～250mg/cm3, (25 DEG C) of heat conductivity no more than 0.025W/mK, burning behavior class height, with hydroxylating glass mat
For reinforcement (mass fraction accounting 5%～60%), aerosil/glass fibre felt composite material is prepared, this is combined
Material has the excellent comprehensive performance of high intensity, low-density, high-flexibility and low heat conductivity.
The purpose of the present invention is realized by following technical measures, wherein the raw material number, is weight unless otherwise specified
Number.
The initiation material of adiabatic aerosil/hydroxylating glass fibre felt composite material is made up of following components：
Based on aerosil, 50～80 parts
Hydroxylating glass mat is used as 70～120 parts of reinforcement.
The preparation method of adiabatic silicon dioxide silica aerogel composite material is comprised the following steps：
1) by deionized water, dehydrated alcohol, hexamethyl disiloxane by weight：18～36 ︰, 230～460 ︰ 0.8～
2.4, in 30～78 DEG C of temperature, after adding molar concentration to be 0.1～0.3 part of the hydrolyst of 0.5～1mol/L, the positive silicon of Deca
208 parts of acetoacetic ester, reacts 0.5～2h, and the Ludox system with MQ structures is obtained, and in sol system, M groups are (CH3)3SiO1/2, Q groups are SiO4/2, 1 ︰ 30～100 of mol ratio of M and Q structures, and through being sufficiently stirred for 2～10h, be obtained with MQ
The Ludox system of structure；
2) hydroxylating process is carried out to glass mat, by glass mat in the acetone soln that concentration is 30%-40%
After middle immersion 30min, deionized water is rinsed, and nitrogen is dried up, to remove the impurity of surface adsorption.By the glass fibre for cleaning
Felt is placed in the mixed solution of 98% concentrated sulphuric acid and 30% hydrogen peroxide, during volume ratio is 3 ︰ 1, in 105 DEG C of reaction 30min of temperature, cold
After take out, deionized water rinsing, nitrogen are dried up, and hydroxylating glass mat is obtained；
3) in step 1) in the Ludox system that obtains, add molar concentration be 0.5～1mol/L gel catalysts 20～
60 parts, by step 2) the hydroxylating glass mat that obtains is immersed in gained Ludox system, in 20～80 DEG C of gels of temperature
Change, then 12～24h of ripening, that is, glass mat-silica wet gel composite is obtained；
4) by step 3) in 500 parts of normal hexane of glass mat and silica wet gel composite, in temperature
Soak is discarded after 20～40 DEG C of 2～10h of immersion treatment, is processed 3 times repeatedly；
5) to step 4) in glass mat and silica wet gel precoated plate after immersion, be 50～120 in temperature
DEG C, pressure is 0.01pa～5pa, and the time is 1～5h；Process is dried, adiabatic aerosil/hydroxylating glass is obtained
Glass fiber felt composite material.
The glass mat is alkali-free glass fibre, and bulk density is 0.1～0.15g/cm3, average fibre diameter is 1
～10 μm, draw ratio meansigma methodss are 10～1000.
The hydrolyst is hydrochloric acid.
The gel catalyst is ammonia.
Structural characterization and performance test：
1st, heat conductivity is tested using GB/T 10294-2008；It is as shown in Table 1 below.
As a result show：Thermal conductivity of composite materials prepared by this method is low, reaches same type of material top standard in the industry.
2nd, combustibility is tested using GB/T 8624-2006；It is as shown in Table 1 below.
As a result show：National A1 levels standard is reached.
The present invention has advantages below：
Hexamethyl disiloxane is adopted for silicon source, and through tetraethyl orthosilicate, is formed and is tied with MQ with a certain proportion of
Structure (proportioning 1：30～Ludox system 100), realizes aeroge system integrally-built modified so as to possess hydrophobic group
Group, based on hydrophobicity provide certain guarantee.
Hydroxylating pretreatment is carried out to glass mat, in composite recombination process, realization makes the hydroxyl in Ludox
There is condensation dehydration in the hydroxyl in base and glass mat, finally realize the chemical bonds of composite material interface, so as to
The bond strength of compound interface is increased, is that the stability of composite is laid a good foundation.
Using negative pressure drying handling process, its process is simple, low cost, process safety are controllable, so as to obtain properties of product
The aerosil heat insulation composite material of good stability, high comprehensive performance.
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to it is pointed out here that be that the present embodiment is served only for
The present invention is further described, but it is not intended that limiting the scope of the invention, the people that is skilled in technique in the field
Member can make the modifications and adaptations of some non-intrinsically safes according to the content of the invention described above to the present invention.
Embodiment 1
The initiation material of adiabatic aerosil/hydroxylating glass fibre felt composite material is made up of following components：
Based on aerosil, 50 parts
Hydroxylating glass mat is used as 70 parts of reinforcement.
The preparation method of adiabatic silicon dioxide silica aerogel composite material is comprised the following steps：
1) by deionized water, dehydrated alcohol, hexamethyl disiloxane it is by mass：18 ︰, 230 ︰ 0.8, in 30 DEG C of temperature,
After molar concentration is added for 0.1 part of the hydrolyst hydrochloric acid of 0.5mol/L, 208 parts of Deca tetraethyl orthosilicate reacts 0.5h, with
In controlling sol system, M groups are (CH3) 3SiO1/2, Q groups are SiO4/2, 1 ︰ 30 of mol ratio of M and Q structures, and through abundant
Stirring 2h, is obtained the Ludox system with MQ structures；
2) hydroxylating process is carried out to glass mat, glass mat is soaked in the acetone soln that concentration is 30%
After 30min, deionized water is rinsed, and nitrogen is dried up, to remove the impurity of surface adsorption.The glass mat for cleaning is placed in
In the mixed solution (volume ratio be 3 ︰ 1) of 98% concentrated sulphuric acid and 30% hydrogen peroxide, in 105 DEG C of reaction 30min of temperature, it is cold after take
Go out, deionized water rinsing, nitrogen are dried up, hydroxylating glass mat is obtained；
3) in step 1) in the Ludox system that obtains, addition molar concentration is 0.5mol/L gel catalysts ammonia 20
Part, by step 2) the hydroxylating glass mat that obtains is immersed in gained Ludox system, in 20 DEG C of gelations of temperature, then
Ripening 12h, that is, be obtained glass mat～silica wet gel composite；
4) by step 3) in 500 parts of normal hexane of glass mat and silica wet gel composite, in temperature
Soak is discarded after 20 DEG C of immersion treatment 2h, is processed 3 times repeatedly；
5) to step 4) in glass mat and silica wet gel precoated plate after immersion, be 50 DEG C in temperature, pressure
Power is 0.01Pa, and the time is 1h；Process is dried, aerosil/hydroxylating glass fibre felt composite material is obtained.
The glass mat is alkali-free glass fibre, and bulk density is 0.1g/cm3, average fibre diameter is 1 μm, long
Footpath is 10 than meansigma methodss.
Embodiment 2
The initiation material of adiabatic aerosil/hydroxylating glass fibre felt composite material is made up of following components：
Based on aerosil, 80 parts
Hydroxylating glass mat is used as 120 parts of reinforcement.
The preparation method of adiabatic silicon dioxide silica aerogel composite material is comprised the following steps：
1) by deionized water, dehydrated alcohol, hexamethyl disiloxane it is by mass：36 ︰, 460 ︰ 2.4, in 78 DEG C of temperature,
After molar concentration is added for 0.3 part of the hydrolyst salt acid+hydrofluoric acid of 1mol/L, 208 parts of Deca tetraethyl orthosilicate reacts 2h,
To control in sol system M groups as (CH3) 3SiO1/2, Q groups are SiO4/2, 1 ︰ 100 of mol ratio of M and Q structures, and pass through
10h is sufficiently stirred for, the Ludox system with MQ structures is obtained；
2) hydroxylating process is carried out to glass mat, glass mat is soaked in the acetone soln that concentration is 40%
After 30min, deionized water is rinsed, and nitrogen is dried up, to remove the impurity of surface adsorption.The glass mat for cleaning is placed in
In the mixed solution (volume ratio be 3 ︰ 1) of 98% concentrated sulphuric acid and 30% hydrogen peroxide, in 105 DEG C of reaction 30min of temperature, it is cold after take
Go out, deionized water rinsing, nitrogen are dried up, hydroxylating glass mat is obtained；
3) in step 1) in the Ludox system that obtains, addition molar concentration is 60 parts of 1mol/L gel catalysts ammonia,
By step 2) the hydroxylating glass mat that obtains is immersed in gained Ludox system, in 80 DEG C of gelations of temperature, Ran Houchen
Change and process 24h, that is, glass mat～silica wet gel composite is obtained；
4) by step 3) in 500 parts of normal hexane of glass mat and silica wet gel composite, in temperature
Soak is discarded after 40 DEG C of immersion treatment 10h, is processed 3 times repeatedly；
5) to step 4) in glass mat and silica wet gel precoated plate after immersion, be 120 DEG C in temperature, pressure
Power is 5Pa, and the time is 5h；Process is dried, aerosil/hydroxylating glass fibre felt composite material is obtained.
The glass mat is alkali-free glass fibre, and bulk density is 0.15g/cm3, average fibre diameter is 10 μm,
Draw ratio meansigma methodss 1000.
Embodiment 3
The initiation material of adiabatic aerosil/hydroxylating glass fibre felt composite material is made up of following components：
Based on aerosil, 65 parts
Hydroxylating glass mat is used as 100 parts of reinforcement.
The preparation method of adiabatic silicon dioxide silica aerogel composite material is comprised the following steps：
1) by deionized water, dehydrated alcohol, hexamethyl disiloxane it is by mass：28 ︰, 400 ︰ 1.5, in 55 DEG C of temperature,
After molar concentration is added for 0.2 part of the hydrolyst hydrochloric acid of 0.75mol/L, 208 parts of Deca tetraethyl orthosilicate reacts 1h, with
In controlling sol system, M groups are (CH3) 3SiO1/2, Q groups are SiO4/2, 1 ︰ 70 of mol ratio of M and Q structures, and through abundant
Stirring 5h, is obtained the Ludox system with MQ structures；
2) hydroxylating process is carried out to glass mat, glass mat is soaked in the acetone soln that concentration is 35%
After 30min, deionized water is rinsed, and nitrogen is dried up, to remove the impurity of surface adsorption.The glass mat for cleaning is placed in
In the mixed solution (volume ratio be 3 ︰ 1) of 98% concentrated sulphuric acid and 30% hydrogen peroxide, in 105 DEG C of reaction 30min of temperature, it is cold after take
Go out, deionized water rinsing, nitrogen are dried up, hydroxylating glass mat is obtained；
3) in step 1) in the Ludox system that obtains, addition molar concentration is 0.8mol/L gel catalysts ammonia 40
Part, by step 2) the hydroxylating glass mat that obtains is immersed in gained Ludox system, in temperature 60 C gelation, then
Ripening 18h, that is, be obtained glass mat-silica wet gel composite；
4) by step 3) in 500 parts of normal hexane of glass mat and silica wet gel composite, in temperature
Soak is discarded after 30 DEG C of immersion treatment 7h, is processed 3 times repeatedly；
5) to step 4) in glass mat and silica wet gel precoated plate after immersion, be 50～100 in temperature
DEG C, pressure is 3Pa, and the time is 3h；Process is dried, aerosil/hydroxylating glass mat composite wood is obtained
Material.
The glass mat is alkali-free glass fibre, and bulk density is 0.12g/cm3, average fibre diameter is 5 μm, long
Footpath is 800 than meansigma methodss.
Table 1 is obtained the performance test of material by embodiment
Claims (5)
1. the preparation method of a kind of adiabatic aerosil/hydroxylating glass fibre felt composite material, it is characterised in that its
Preparation method is comprised the following steps：
1) by deionized water, dehydrated alcohol, hexamethyl disiloxane it is by mass：18～36 ︰, 230～460 ︰ 0.8～2.4,
In 30～78 DEG C of temperature, after adding molar concentration to be 0.1～0.3 part of the hydrolyst of 0.5～1mol/L, the positive silicic acid second of Deca
208 parts of ester, reacts 0.5～2h, to control in sol system M groups as (CH3)3SiO1/2, Q groups are SiO4/2, M and Q structures
1 ︰ 30～100 of mol ratio, and through being sufficiently stirred for 2～10h, the Ludox system with MQ structures is obtained；
2) hydroxylating process is carried out to glass mat, glass mat is soaked in acetone soln of the concentration for 30%-40%
After bubble 30min, deionized water is rinsed, and nitrogen is dried up, to remove the impurity of surface adsorption；The glass mat for cleaning is put
In 98% concentrated sulphuric acid and the mixed solution of 30% hydrogen peroxide, during volume ratio is 3 ︰ 1, in 105 DEG C of reaction 30min of temperature, it is cold after take
Go out, deionized water rinsing, nitrogen are dried up, hydroxylating glass mat is obtained；
3) in step 1) in the Ludox system that obtains, addition molar concentration is 20～60 parts of 0.5～1mol/L gel catalysts,
By step 2) the hydroxylating glass mat that obtains is immersed in gained Ludox system, in 20～80 DEG C of gelations of temperature, so
12～24h of ripening, that is, be obtained glass mat-silica wet gel composite afterwards；
4) by step 3) in 500 parts of normal hexane of glass mat and silica wet gel composite, temperature 20～
Soak is discarded after 40 DEG C of 2～10h of immersion treatment, is processed 3 times repeatedly；
5) to step 4) in glass mat and silica wet gel precoated plate after immersion, be 50～120 DEG C in temperature, pressure
Power is 0.01Pa～5Pa, and the time is 1～5h；Process is dried, aerosil/hydroxylating glass mat is obtained
Composite；
Wherein, the initiation material of the composite is made up of following components, by weight：Based on aerosil
50～80 parts, hydroxylating glass mat is used as 70～120 parts of reinforcement.
2. the preparation method of adiabatic aerosil/hydroxylating glass fibre felt composite material according to claim 1,
It is characterized in that the glass mat is alkali-free glass fibre, bulk density is 0.1～0.15g/cm3, average fibre diameter
For 1～10 μm, draw ratio average out to 10～1000.
3. the preparation method of adiabatic aerosil/hydroxylating glass fibre felt composite material according to claim 1,
It is characterized in that hydrolyst is hydrochloric acid.
4. the preparation method of adiabatic aerosil/hydroxylating glass fibre felt composite material according to claim 1,
It is characterized in that gel catalyst is ammonia.
5. the preparation method of adiabatic aerosil/hydroxylating glass fibre felt composite material according to claim 1
The adiabatic aerosil for preparing/hydroxylating glass fibre felt composite material.
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| KR102193438B1 (en) * | 2017-11-16 | 2020-12-21 | 주식회사 엘지화학 | Silica aerogel blanket with low dust and method for preparing the same |
| CN108101500A (en) * | 2017-12-06 | 2018-06-01 | 吕莉 | A kind of preparation method of high intensity spider silk dioxide composite silica aerogel |
| CN108358459A (en) * | 2018-05-10 | 2018-08-03 | 天长市天意玻璃制品有限公司 | A kind of preparation method of resistance to compression heat-protecting glass fibrous composite |
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| CN110950629A (en) * | 2018-09-27 | 2020-04-03 | 北京聚能三晶科技有限公司 | Silica aerogel composite thermal insulation material and preparation method thereof |
| CN110106695B (en) * | 2019-04-14 | 2022-06-21 | 泰州浩纳新材料科技有限公司 | Silica nanometer heat-preservation heat-insulation felt |
| CN111535019A (en) * | 2020-04-21 | 2020-08-14 | 浙江岩谷科技有限公司 | Preparation method of hydrophobic glass fiber felt-silica aerogel heat insulation composite material |
| CN111592329B (en) * | 2020-05-25 | 2022-06-03 | 福建拓烯新材料科技有限公司 | Preparation method of modified silica aerogel and modified silica aerogel |
| CN114851649A (en) * | 2022-05-17 | 2022-08-05 | 浙江联洋新材料股份有限公司 | Ultra-wide breadth glass fiber fabric and preparation method thereof |
| CN114988904A (en) * | 2022-05-19 | 2022-09-02 | 中国科学院金属研究所 | Preparation method for realizing ultralow-density and ultralow-heat-conductivity carbon aerogel composite material through surface functionalization of cotton fibers |
| CN115012208A (en) * | 2022-06-28 | 2022-09-06 | 武汉中科先进材料科技有限公司 | Efficient normal-pressure drying large-scale preparation method of silica aerogel felt |
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| DE4430642A1 (en) * | 1994-08-29 | 1996-03-07 | Hoechst Ag | Airgel and xerogel composites, processes for their production and their use |
| IL119432A0 (en) * | 1996-10-16 | 1997-01-10 | I R D Fuel Technologies Ltd | Filter for separating water from fuel |
| CN102557577B (en) * | 2011-11-01 | 2014-03-19 | 厦门纳美特新材料科技有限公司 | Preparation method of silicon dioxide aerogel composite material |
| CN104496403B (en) * | 2014-12-23 | 2017-02-22 | 南京唯才新能源科技有限公司 | Reinforced aerogel composite material and preparation method thereof |
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