CN105236912A - Composite fiber-reinforced hydrophobic SiO2 aerogel and preparation method thereof - Google Patents
Composite fiber-reinforced hydrophobic SiO2 aerogel and preparation method thereof Download PDFInfo
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- CN105236912A CN105236912A CN201510549062.2A CN201510549062A CN105236912A CN 105236912 A CN105236912 A CN 105236912A CN 201510549062 A CN201510549062 A CN 201510549062A CN 105236912 A CN105236912 A CN 105236912A
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Abstract
The invention belongs to the field of advanced composite materials and particularly relates to a composite fiber-reinforced hydrophobic SiO2 aerogel and a preparation method thereof. In the method, a proper silicon source is employed as a precursor and a sol-gel method is employed. The method includes the following steps: 1) fully mixing pre-treated composite fibers with sol, performing aging treatment and performing surface modification; 2) connecting a hydrophobic group on the surface of the gel to achieve a hydrophobic effect; 3) replacing the solvent, such as ethanol, water and the like which are high in surface tension, with a low-surface-tension solvent through solvent replacement to reduce capillary tension in the liquid during drying, thereby reducing the phenomenon of gel collapse caused by evaporation of the solvent during a normal-pressure drying process; and 4) performing the normal-pressure drying process to prepare the hydrophobic SiO2 aerogel composite material. The method is simple and quick, is reduced in production cost, can improve both the strength and toughness of the composite aerogel and broadens the application of SiO2 aerogel on surfaces of irregular-shaped objects.
Description
Technical field
The invention belongs to advanced composite material field, be specifically related to a kind of conjugated fibre and strengthen hydrophobic SiO
2aerogel and preparation method thereof.
Background technology
SiO
2aerogel is a kind of nano-meter porous amorphous body material with three-dimensional net structure.This special structure makes it have specific surface area up to 1000m
2/ g, density is low to moderate 3kg/m
3, porosity is up to 99.8% (its pore dimension and colloidal particle size are respectively in 1-100nm and 2-60nm), and the performance such as ultralow thermal conductivity 0.015W/ (mK).The performance of numerous excellence makes it be applied in various fields such as aerospace, chemical industry, electrochemistry, metallurgy.
In recent years, due to pure SiO
2aerogel density is low and porosity is high causes its poor mechanical property, and as low in intensity, poor toughness etc., can not separately for heat insulating engineering.Under the prerequisite not affecting effect of heat insulation, improve the study hotspot that Mechanical Properties of Aerogels becomes aerogel field gradually.Research mainly concentrates on the flexibility how realizing aerogel, namely under the prerequisite ensureing high strength, solves the high problem of aerogel fragility simultaneously.
Conjugated fibre strengthens aerogel and mainly adopts sol-gel method to prepare.ZHANG etc. adopt interpolation glass fibre to prepare SiO
2aerogel material, but glass fibre fragility is larger, makes prepared glass fiber reinforcement aerogel material rigidity large, flexible poor.Ni Wen etc. adopt English afwillite to strengthen preparation SiO
2aerogel composite, its bending strength is 0.18MPa, but prepared aerogel can not have good intensity and toughness effect simultaneously.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, object is to provide a kind of conjugated fibre to strengthen hydrophobic SiO
2aerogel and preparation method thereof.
For achieving the above object, the technical solution adopted in the present invention is:
A kind of conjugated fibre strengthens hydrophobic SiO
2the preparation method of aerogel, is characterized in that, comprises the steps:
(1) preparation of silicon sol: be 1:4 ~ 6:3 ~ 4:0.47 mixing in molar ratio by tetraethoxy, dehydrated alcohol, deionized water and methane amide, after abundant stirring, add salt acid for adjusting pH value to 3 ~ 4, be heated to 50 DEG C ~ 60 DEG C fully to stir, sealing preservation one day, add ammoniacal liquor again and regulate pH to 6 ~ 8, obtain silicon sol;
(2) compound of silicon sol and fiber and aging: slowly pour into after the silicon sol prepared by step (1) is stirred in the container being filled with conjugated fibre and leave standstill, formed after wet gel until silicon sol, add the surface that dehydrated alcohol covers wet gel, and use preservative film sealed mold, allow wet gel seal aging;
(3) finishing of wet gel: be immersed in surface-modifying agent by the wet gel after aging for step (2) and carry out gel surface hydrophobically modified, described surface-modifying agent is the mixing solutions of trimethylchlorosilane and normal hexane;
(4) solvent exchange of wet gel: add the little solvent of surface tension and carry out solvent soaking displacement in the wet gel of step (3) after surface modification, make deionized water residual in wet gel hole and dehydrated alcohol out replaced;
(5) constant pressure and dry: the wet gel after being replaced by step (4) solvent soaking carries out constant pressure and dry, obtains conjugated fibre and strengthens hydrophobic SiO2 aerogel.
In such scheme, the volume ratio of step (2) described conjugated fibre and silicon sol is 1:1 ~ 1.5.
In such scheme, step (2) described conjugated fibre is composited in the ratio of 1:1 ~ 2 by mullite fiber and polyster fibre; Further, before described conjugated fibre uses, low-concentration hcl is adopted to carry out 2 ~ 4h dipping pretreatment to step (2) described conjugated fibre.
In such scheme, the add-on of step (2) described dehydrated alcohol is 1/5 ~ 1/3 of the volume of wet gel, and the described aging time is 24h ~ 48h.
In such scheme, the volume ratio of step (3) described surface-modifying agent and wet gel is 1 ~ 2:1; The volume ratio of described trimethylchlorosilane and normal hexane is 1:7 ~ 10.
In such scheme, step (4) described solvent is dehydrated alcohol or normal hexane, and the volume ratio of described solvent and wet gel is 1 ~ 2:1, and the number of times of described solvent soaking displacement is 2 ~ 4 times, and the time of each solvent soaking displacement is 12 ~ 24h.
In such scheme, step (5) described constant pressure and dry is 50 DEG C ~ 60 DEG C, 12h ~ 24h; 90 DEG C, 12h ~ 24h; 120 DEG C, 6h ~ 24h.
The conjugated fibre that above-mentioned preparation method prepares strengthens hydrophobic SiO
2aerogel.
Beneficial effect of the present invention is as follows: the present invention with suitable silicon source for presoma, adopt sol-gel method, after the conjugated fibre handled well is fully mixed with colloidal sol, carry out burin-in process, then finishing is carried out, hydrophobic grouping is connected in gel surface, reach hydrophobic effect, and adopt by solvent exchange the ethanol that in the solvent exchange gel that surface tension is little, surface tension is large, water equal solvent, capillary tension when reducing dry between liquid, thus reduce in constant pressure and dry process because solvent evaporates the phenomenon causing gel to subside, finally carry out constant pressure and dry, prepare a kind of hydrophobic SiO
2aerogel composite, conjugated fibre of the present invention strengthens hydrophobic SiO
2the density of aerogel is low to moderate 0.225g/cm
3, volumetric shrinkage is little, and specific surface area is up to 878.554m
2/ g, and there is certain hydrophobic effect, reach the effect of hydrophobically modified, and mechanical property significantly improves, folding strength reaches 1.53MPa, and ultimate compression strength reaches 1.7MPa, significantly improves the toughness of material under the intensity prerequisite ensureing matrix material, (2) the method for the invention simple and fast, improves intensity and the toughness of composite aerogel, expands SiO while reducing production cost
2aerogel is in the application of irregular article surface.
Accompanying drawing explanation
Fig. 1 is be that conjugated fibre prepared by embodiment 1 strengthens hydrophobic SiO
2aerogel pictorial diagram.
Fig. 2 is the SiO of long time without surface modification treatment
2conjugated fibre prepared by aerogel and embodiment 2 strengthens hydrophobic SiO
2the ftir analysis figure of aerogel.
Embodiment
In order to understand the present invention better, illustrate content of the present invention further below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
Embodiment 1
A kind of conjugated fibre strengthens hydrophobic SiO
2the preparation method of aerogel, comprises the steps:
(1) preparation of silicon sol: by 10.8g tetraethoxy, 9.2g dehydrated alcohol, 3.6g deionized water and 1.4g methane amide short mix, after abundant stirring, add between a certain amount of salt acid for adjusting pH value to 3-4, be heated to 60 DEG C and fully stir 90min, sealing preservation allows it fully be hydrolyzed in one day, adding a certain amount of ammoniacal liquor after hydrolysis regulates pH between 6-8, obtains silicon sol;
(2) compound of silicon sol and fiber aging: slowly pour into after being stirred by the silicon sol prepared by step (1) in the container being filled with conjugated fibre (described conjugated fibre is composited in the ratio of 1:1 by mullite fiber and polyster fibre) and leave standstill, the volume ratio of described conjugated fibre and silicon sol is 1:1; Formed after wet gel until silicon sol, at the dehydrated alcohol of wet gel surface coverage 20ml, volume is 1/3 of wet gel, uses preservative film sealed vessel, makes gel seal aging, and digestion time is 24 hours;
(3) finishing of wet gel: the wet gel after aging for step (2) is immersed in 7.5ml trimethylchlorosilane and 52.5ml normal hexane mixed solution and carries out surface modification, be modified as 48 hours, change modification liquid twice therebetween;
(4) solvent exchange of wet gel: wet gel modified in step (3) pours a small amount of normal hexane into and carries out surface cleaning, pour out scavenging solution and again pour the normal hexane being about wet gel volume 2 times into, immersion displacement is carried out in sealing, soaking number of times is 2 times, and each soak time is 12 hours;
(5) constant pressure and dry: by the wet gel after step (4) solvent exchange 50 DEG C of dryings 12 hours, at 90 DEG C, drying 12 hours, 120 DEG C of dryings 6 hours, obtains conjugated fibre and strengthens hydrophobic SiO after naturally cooling to room temperature
2aerogel.
The conjugated fibre that the present embodiment prepares strengthens hydrophobic SiO
2the pictorial diagram of aerogel is shown in Fig. 1, and diameter is about 10cm, and apparent density is 0.259cm
3/ g, porosity is 74.97%, specific surface area 683.713m
2/ g, folding strength is 0.89MPa, and ultimate compression strength is 0.91MPa.
Embodiment 2
A kind of conjugated fibre strengthens hydrophobic SiO
2the preparation method of aerogel, comprises the steps:
(1) preparation of silicon sol: by 10.8g tetraethoxy, 13.2g dehydrated alcohol, 3.6g deionized water and 1.4 methane amide short mix, after abundant stirring, add between a certain amount of salt acid for adjusting pH value to 3-4, be heated to 50 DEG C and fully stir 90min, sealing preservation allows it fully be hydrolyzed in one day, adding a certain amount of ammoniacal liquor after hydrolysis regulates pH between 6-8, obtains silicon sol;
(2) compound of silicon sol and fiber aging: (described conjugated fibre is composited in the ratio of 1:1.5 by mullite fiber and polyster fibre slowly to pour the conjugated fibre that is filled with of anticipating after being stirred by the silicon sol prepared by step (1) into, adopt low-concentration hcl 2h ~ 4h dipping pretreatment is carried out to conjugated fibre) container in leave standstill, the volume ratio of described conjugated fibre and silicon sol is 1:1.5; Formed after wet gel until silicon sol, at the dehydrated alcohol of wet gel surface coverage 10ml, volume is 1/5 of wet gel, uses preservative film sealed vessel, makes gel seal aging, and digestion time is 48 hours;
(3) finishing of wet gel: the wet gel after aging for step (2) is immersed in 5ml trimethylchlorosilane and 45ml normal hexane mixed solution and carries out surface modification, be modified as 48 hours, change modification liquid twice therebetween;
(4) solvent exchange of wet gel: the wet gel that modification is complete in step (3) pours a small amount of normal hexane into and carries out surface cleaning, pour out scavenging solution and again pour the normal hexane being about wet gel volume 1 times into, immersion displacement is carried out in sealing, soaking number of times is 3 times, and each soak time is 18 hours;
(5) constant pressure and dry: by the wet gel after step (4) solvent exchange 60 DEG C of dryings 24 hours, at 90 DEG C, drying 24 hours, 120 DEG C of dryings 12 hours, obtains conjugated fibre and strengthens hydrophobic SiO after naturally cooling to room temperature
2aerogel.
Fig. 2 is that the conjugated fibre of long time without surface modification treatment strengthens SiO
2conjugated fibre prepared by aerogel and embodiment 2 strengthens hydrophobic SiO
2the ftir analysis figure of aerogel.Fig. 2-a curve is that the conjugated fibre of long time without surface modification strengthens SiO
2the infrared absorption line of aerogel, at 1633cm in this spectral line
-1neighbouring absorption peak is the flexural vibration of H-OH, at 3431cm
-1the neighbouring peak occurred is-OH asymmetrical stretching vibration, and in figure, b curve is the conjugated fibre enhancing SiO through surface modification
2the infrared absorption line of aerogel, spectral line is at 3433cm
-1neighbouring-OH absorption peak weakens to some extent, meanwhile, and 958cm
-1near represent Si-OH stretching vibration absorption peak almost disappear, show that the hydrophilic radical of aerogel obviously reduces; And at 2965cm
-1and 1257cm
-1, 848cm
-1the neighbouring peak occurred is respectively the asymmetric vibration of C-H and the rocking vibration of Si-C, in addition, and 759cm in figure
-1the peak that place occurs is Si-CH
3symmetrical stretching vibration, it can be said that bright conjugated fibre strengthen SiO
2aerogel is after surface modification, and its surperficial major part-OH is by-CH
3replacing, aerogel surface is by hydrophobic grouping in modification.
The conjugated fibre that the present embodiment prepares strengthens hydrophobic SiO
2the pictorial diagram of aerogel is shown in Fig. 1, and diameter is about 10cm, and apparent density is 0.225cm
3/ g, porosity is 82.88%, and specific surface area is 878.554m
2/ g, folding strength is 1.53MPa, and ultimate compression strength is 1.7MPa.
Embodiment 3
A kind of conjugated fibre strengthens hydrophobic SiO
2the preparation method of aerogel, comprises the steps:
(1) preparation of silicon sol: by 10.8g tetraethoxy, 13.2g dehydrated alcohol, 2.7g deionized water and 1.4g methane amide short mix, after abundant stirring, add between a certain amount of salt acid for adjusting pH value to 3-4, be heated to 60 DEG C and fully stir 90min, sealing preservation allows it fully be hydrolyzed in one day, adding a certain amount of ammoniacal liquor after hydrolysis regulates pH between 6-8, obtains silicon sol;
(2) compound of silicon sol and fiber aging: slowly pour being filled with in the container of conjugated fibre (described conjugated fibre is composited in the ratio of 1:2 by mullite fiber and polyster fibre) of anticipating after being stirred by the silicon sol prepared by step (1) into and leave standstill, the volume ratio of described conjugated fibre and silicon sol is 1:1; Formed after wet gel until silicon sol, at the dehydrated alcohol of wet gel surface coverage 10ml, volume is 1/5 of wet gel, uses preservative film sealed vessel, makes gel seal aging, and digestion time is 24 hours;
(3) finishing of wet gel: the wet gel after aging for step (2) is immersed in 3ml trimethylchlorosilane and 27ml normal hexane mixed solution and carries out surface modification, be modified as 48 hours, change modification liquid twice therebetween;
(4) solvent exchange of wet gel: wet gel modified in step (3) pours a small amount of normal hexane into and carries out surface cleaning, pour out scavenging solution and again pour the normal hexane being about wet gel volume 2 times into, immersion displacement is carried out in sealing, soaking number of times is 4 times, and each soak time is 24 hours;
(5) constant pressure and dry: by the wet gel after step (4) solvent exchange 50 DEG C of dryings 24 hours, at 90 DEG C, drying 24 hours, 120 DEG C of dryings 24 hours, obtains conjugated fibre and strengthens hydrophobic SiO after naturally cooling to room temperature
2aerogel.
The conjugated fibre that the present embodiment prepares strengthens hydrophobic SiO
2the pictorial diagram of aerogel is shown in Fig. 1, and diameter is about 10cm, and apparent density is 0.27cm
3/ g, porosity is 79.97%, specific surface area 712.353m
2/ g, folding strength is 1.1MPa, and ultimate compression strength is 1.15MPa.
Obviously, above-described embodiment is only for the example done clearly is described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And therefore amplified apparent change or variation are still in the protection domain of the invention.
Claims (9)
1. a conjugated fibre strengthens hydrophobic SiO
2the preparation method of aerogel, is characterized in that, comprises the steps:
(1) preparation of silicon sol: be 1:4 ~ 6:3 ~ 4:0.47 mixing in molar ratio by tetraethoxy, dehydrated alcohol, deionized water and methane amide, after abundant stirring, add salt acid for adjusting pH value to 3 ~ 4, be heated to 50 DEG C ~ 60 DEG C fully to stir, sealing preservation one day, add ammoniacal liquor again and regulate pH to 6 ~ 8, obtain silicon sol;
(2) compound of silicon sol and fiber and aging: slowly pour into after the silicon sol prepared by step (1) is stirred in the container being filled with conjugated fibre and leave standstill, formed after wet gel until silicon sol, add the surface that dehydrated alcohol covers wet gel, and use preservative film sealed mold, allow wet gel seal aging;
(3) finishing of wet gel: be immersed in surface-modifying agent by the wet gel after aging for step (2) and carry out gel surface hydrophobically modified, described surface-modifying agent is the mixing solutions of trimethylchlorosilane and normal hexane;
(4) solvent exchange of wet gel: add the little solvent of surface tension and carry out solvent soaking displacement in the wet gel of step (3) after surface modification, make deionized water residual in wet gel hole and dehydrated alcohol out replaced;
(5) constant pressure and dry: the wet gel after being replaced by step (4) solvent soaking carries out constant pressure and dry, obtains conjugated fibre and strengthens hydrophobic SiO
2aerogel.
2. preparation method according to claim 1, is characterized in that, the volume ratio of step (2) described conjugated fibre and silicon sol is 1:1 ~ 1.5.
3. preparation method according to claim 1, is characterized in that, step (2) described conjugated fibre is composited in the ratio of 1:1 ~ 2 by mullite fiber and polyster fibre.
4. preparation method according to claim 3, is characterized in that, adopts low-concentration hcl to carry out 2 ~ 4h dipping pretreatment to step (2) described conjugated fibre.
5. preparation method according to claim 1, is characterized in that, the add-on of step (2) described dehydrated alcohol is 1/5 ~ 1/3 of the volume of wet gel, and the described aging time is 24h ~ 48h.
6. preparation method according to claim 1, is characterized in that, the volume ratio of step (3) described surface-modifying agent and wet gel is 1 ~ 2:1; The volume ratio of described trimethylchlorosilane and normal hexane is 1:7 ~ 10.
7. preparation method according to claim 1, it is characterized in that, step (4) described solvent is dehydrated alcohol or normal hexane, and the volume ratio of described solvent and wet gel is 1 ~ 2:1, the number of times of described solvent soaking displacement is 2 ~ 4 times, and the time of each solvent soaking displacement is 12 ~ 24h.
8. preparation method according to claim 1, is characterized in that, step (5) described constant pressure and dry is 50 DEG C ~ 60 DEG C, 12h ~ 24h; 90 DEG C, 12h ~ 24h; 120 DEG C, 6h ~ 24h.
9. the conjugated fibre that the arbitrary described preparation method of claim 1 ~ 8 prepares strengthens hydrophobic SiO
2aerogel.
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| CN106431168A (en) * | 2016-09-29 | 2017-02-22 | 成都新柯力化工科技有限公司 | Method for preparing bulk-shaped flexible aerogel through normal-pressure drying |
| CN106565224A (en) * | 2016-10-18 | 2017-04-19 | 成都新柯力化工科技有限公司 | Method for improving silica aerogel by using mullite fibers |
| CN106747576A (en) * | 2016-11-22 | 2017-05-31 | 成都新柯力化工科技有限公司 | A kind of method that normal pressure homogenizing low cost prepares aeroge for building |
| CN107662923A (en) * | 2017-10-19 | 2018-02-06 | 加新科技(深圳)有限公司 | A kind of continuous boron for preparing adulterates SiO2The method of aeroge |
| CN108221367A (en) * | 2018-03-21 | 2018-06-29 | 青岛纳博科环保科技有限公司 | Hydrophobic modifier for activated carbon fibre and preparation method thereof, hydrophobic active Carbon fibe and preparation method thereof |
| CN108468907A (en) * | 2018-04-20 | 2018-08-31 | 宿迁南航新材料与装备制造研究院有限公司 | A kind of vacuum heat-insulating plate and preparation method thereof of fiber reinforcement nano-powder material |
| CN109210319A (en) * | 2018-11-12 | 2019-01-15 | 中研信源（北京）节能科技有限公司 | A kind of aerogel vacuum thermal insulation plate and its core material with and preparation method thereof |
| CN110918011A (en) * | 2019-12-09 | 2020-03-27 | 东北林业大学 | SiO (silicon dioxide)2Preparation method and application of/glass fiber composite aerogel |
| CN111302760A (en) * | 2018-12-11 | 2020-06-19 | 天津大学 | Mullite whisker/fiber synergistically enhanced silica aerogel multi-scale composite structure and preparation method and application thereof |
| CN112079618A (en) * | 2020-09-14 | 2020-12-15 | 南京工业大学 | Preparation method of modified silica aerogel heat insulation sheet |
| CN113816387A (en) * | 2021-05-16 | 2021-12-21 | 响水华夏特材科技发展有限公司 | Efficient preparation method and application of aerogel material |
| CN117654466A (en) * | 2024-02-01 | 2024-03-08 | 浙江新和成股份有限公司 | Catalyst, process for producing the same, process for producing ethylenically unsaturated acid or ester thereof |
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| CN108221367A (en) * | 2018-03-21 | 2018-06-29 | 青岛纳博科环保科技有限公司 | Hydrophobic modifier for activated carbon fibre and preparation method thereof, hydrophobic active Carbon fibe and preparation method thereof |
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| CN111302760A (en) * | 2018-12-11 | 2020-06-19 | 天津大学 | Mullite whisker/fiber synergistically enhanced silica aerogel multi-scale composite structure and preparation method and application thereof |
| CN110918011A (en) * | 2019-12-09 | 2020-03-27 | 东北林业大学 | SiO (silicon dioxide)2Preparation method and application of/glass fiber composite aerogel |
| CN112079618A (en) * | 2020-09-14 | 2020-12-15 | 南京工业大学 | Preparation method of modified silica aerogel heat insulation sheet |
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